Insecticidal compositions and methods of using the same

ABSTRACT

Insecticidal compositions have at least one active agent and at least one insecticide. The active agent can include  perilla  oil, a component found in  perilla  oil, or a perillaldehyde or carvone analog. The insecticide can include a pyrethrum, pyrethrin, pyrethroid, neonicotinoid, chlofenapyr, ethiprole, sulfoxoflor, carbamate, organophosphate, or organochlorine. Methods for controlling insects include contacting an insect with an effective amount of a composition described in this specification. Modified plants that produce an active agent can be contacted with an insecticide.

CROSS-REFERENCE TO RELATED APPLICATIONS

This application is a continuation of U.S. patent application Ser. No.13/548,998, filed Jul. 13, 2012, which claims the benefit of priority toco-pending U.S. Provisional Patent Application No. 61/507,557 filed onJul. 13, 2011, 61/543,180, filed on Oct. 4, 2011, and 61/580,427, filedon Dec. 27, 2011. The entire contents of each of these applications areincorporated into this specification by reference in their entireties.

FIELD

This specification relates to compositions and methods useful for insectcontrol.

BACKGROUND

Many types of insecticides have been used to kill mosquitoes and otherinsect pests. Nevertheless, many insecticides have disadvantages. Someinsecticides are toxic to humans, are harmful to the environment, orhave limited efficacy. Further, there is an increasing demand forcompositions containing naturally occurring or so-called organiccompounds. Accordingly, there is a continuing need for organic compoundshaving improved insecticidal properties, while being substantiallynon-toxic or only mildly toxic to humans.

Certain plant species produce essential oils that serve as naturalsources of insect repellents, insecticides, fragrances, or other usefulchemicals. For example, perilla oil and certain of its components havebeen used in a variety of applications, including in varnishes, in theproduction of inks and linoleums, and in the culinary field as amarinade.

Perilla oil is extracted from annual herbs belonging to the genusPerilla through several methods, including but not limited to coldpressing of the seeds or steam distillation of the leaves. Two types ofperilla oil are available, seed and leaf extracts. The major componentof perilla seed extract is linolenic acid, and the major components ofperilla leaf extract are perillaldehyde, limonene, β-caryophyllene, andfarnesene.

SUMMARY

This specification demonstrates the ability of perilla oil and some ofits components to act as a synergist of insecticides such as pyrethrum,pyrethrins, pyrethroids, spinosad, neonicotinoids, sulfoxoflor,carbamates, organophosphates, and organochlorines. The disclosure alsodemonstrates that perilla oil, perilla oil components, and certainperillaldehyde and carvone analogs can be used as synergists forinsecticides in certain compositions. The disclosure furtherdemonstrates that certain compounds having a modified cyclohexene ringcontaining a substituted or unsubstituted methyl group can be used assynergists for insecticides in certain compositions.

In some aspects, an insecticidal composition is provided comprising aninsecticide and an active agent present in an amount of about 1% to 99%(by weight) of the composition. The active agent can be perilla oil, aperilla oil component, or a perillaldehyde or carvone analog. Forexample, the active agent can be selected from the group consisting offarnesene, perillaldehyde, linolenic acid, caryophyllene, limonene(including D-limonene), carvone, perillyl alcohol, pinene, linalool,germacrene, bergamotene, and spathulenol, or the active agent can beselected from the group consisting of limonene (including D-limonene),perillyl alcohol (including (S)-(−)-perillyl alcohol), perillic acid(including (S)-(−)-perillic acid), myrtenal (including(1R)-(−)-myrtenal), and 3-methyl-1-cyclohexene-1-carboxaldehyde. Theactive agent can also be any combination of these perilla oil componentsand perillaldehyde or carvone analogs.

In some embodiments, the active agent is a compound of Formula (I):

wherein:

R¹ is selected from the group consisting of —CH₂OH, —CHO, and —COOR^(a);

R² is selected from the group consisting of hydrogen, alkyl, andalkenyl;

R³ is selected from the group consisting of hydrogen and alkyl;

R⁴ is hydrogen, or R⁴ and R² are taken together with the atoms to whichthey are attached to form an optionally substituted ring; and

R^(a) is selected from the group consisting of hydrogen and alkyl.

The insecticide in the compositions can be present at less than about95% by weight, less than about 60% by weight or in other amounts asdescribed is this specification and can comprise one or more of apyrethrin, pyrethroid, neonicotinoid, chlofenapyr, ethiprole,sulfoxoflor, carbamate, organophosphate, or organochlorine. Examples ofpyrethrin include one or more of jasmolin-I, cinerin-I, pyrethrin-I,jasmolin-II, cinerin-II, or pyrethrin-II. Examples of pyrethroid includeone or more of etofenprox, permethrin, prallethrin, resmethrin,sumithrin, allethrin, alpha-cypermethrin, bifenthrin, beta-cypermethrin,cyfluthrin, cypermethrin, deltamethrin, esfenvalerate, etofenprox,lamdba-cyhalothrin, or zeta-cypermethrin. Examples of neonicotinoidsinclude one or more of dinotefuran, acetamiprid, clothianidin,imidacloprid, nitenpyram, thiacloprid, or thiamethoxam. The compositioncan be substantially free of piperonyl butoxide, N-octyl bicycloheptenedicarboximide, or both.

In some aspects, the composition includes one or more of mineral oil,glycerol, or a diluent that provides viscosity modifying properties. Thecomposition can be formulated to be suitable for application as anaerosol, fog, mist, spray, vapor, ultra low volume spray (ULV), surfacecontact treatment, or a combination thereof.

In other aspects, a method for controlling insects is provided, in whicha population of insects, such as mosquitoes, is contacted with aneffective amount of a composition described in this specification. Thepopulation of insects can be controlled by topically applying thecomposition to the population in an amount sufficient to kill at least25%, 50%, or any proportion disclosed in this specification of thepopulation. The composition can be applied by aerosol or as a mist, fog,vapor, spray, ULV spray, or surface contact treatment or as acombination of any of these methods.

In other aspects, a method for controlling insect pests on a plant isprovided by contacting a transgenic plant with an insecticide or anactive agent selected from the group consisting of (i) perilla oil; (ii)a perilla oil component selected from the group consisting of farnesene,perillaldehyde, linolenic acid, caryophyllene, limonene, carvone,perillyl alcohol, pinene, linalool, germacrene, bergamotene, andspathulenol; and (iii) a perillaldehyde or carvone analog. Thetransgenic plant can be modified to heterologously express an activeagent, such as at least one of farnesene, perillaldehyde, linolenicacid, caryophyllene, limonene, carvone, perillyl alcohol, pinene,linalool, germacrene, bergamotene, and spathulenol, which is expressedin an amount sufficient to have a synergistic effect on insecticidalactivity, or the transgenic plant can be modified to heterologouslyexpress an insecticide and contacted with the active agent in an amountsufficient to have a synergistic effect on insecticidal activity.

In other aspects, a method for controlling insect pests on a plantincludes the step of contacting a transgenic plant heterologouslyproducing an insecticide and an active agent selected from at least oneof the group consisting of farnesene, perillaldehyde, linolenic acid,caryophyllene, limonene, carvone, perillyl alcohol, pinene, linalool,germacrene, bergamotene, and spathulenol with a population of insectpests. The active agent has a synergistic effect on insecticidalactivity in the plant and controls the insect pests.

Other aspects of the disclosure will become apparent by consideration ofthe detailed description and accompanying drawings.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 is a schematic representation of the experimental setup for thefield study described in Example 58.

FIG. 2 is a chart showing the activity of P450 cytochrome enzyme (P450)in the presence or absence of inhibitors as described in Example 59. Thecontrol treatment contained acetone; piperonyl butoxide (PBO), a knowncytochrome P450 inhibitor, was used as a positive control. The chartshows the inhibition potency of perillaldehyde (perilla) when present at1% and 10%.

DETAILED DESCRIPTION

This specification broadly relates to insecticidal compositions andmethods of using the same. The compositions and methods are effectiveand selective in killing insects. This invention describes the use ofperilla oil, its components, or other related compounds to synergize theactivity of non-perilla-oil-related insecticides. Accordingly, for thepurposes of this specification, an insecticide refers to a compoundhaving insecticidal activity, other than perilla oil, one of itscomponents, a perillaldehyde analog, or the other related synergistsdescribed in this specification.

In some embodiments, an active agent comprises perilla oil, one of itscomponents, or a perillaldehyde analog. Perilla oil, perilla oilcomponents, and perillaldehyde analogs can be extracted from plantsources or can be synthesized. Parts of the plant used to extract thesecompounds include, but are not limited to, at least one of the flower,stem, leaf, seed, fruit, or fruit peel of the plant.

Plant sources may include plants of the genus Perilla, including, butnot limited to, green varieties—Perilla frutescens (L.) Britt. var.crispa, var. arguta, var. arcuta, var. stricta, Perilla ocymoides L. andPerilla crispa var. ocymoides—and the purple leaf varieties—Perillafrutescens var. acuta, var. typica, var. stricta, var. crisp, var.atropurpurea, var. crispa, var. nankinensis, var. olifera, var.japonica, var. citriodora, Perilla crispa (Thunb.), and Perillanankinensis (Lour.).

Perilla oil can be extracted from a plant by any means known in the art,including, but not limited to, at least one of pressing, grinding,mashing, distillation such as steam distillation, cold pressureextraction, chromatography, a suitable solvent extraction such as liquidCO₂ extraction, and methanol extraction of a part or combination ofparts of the plant source.

Perilla oil components and certain perillaldehyde analogs may be derivedor isolated (e.g., extracted) from perilla oil or from a plant source,as described above. Perillaldehyde, a component of perilla oil, can alsobe extracted from other plant sources outside of the genus Perillaincluding, but not limited to, Sium latifolium, Citrus reticulata (e.g.,the peels of the fruit), Limnophila geoffrayi, Laser tribolium,Limnophiliz aromatica, Laserpitium siler, Conyza newii, Cuminum cyminum,and Plectranthus marruboides. (R)-carvone can be extracted from perillaoil and other plant sources including artemisa fergamensis, bergamot,cassis, chamomile moroccan wild, clove oil, eucalyptus globulus,gingergrass, grapefruit, juniperberry, lavender, lemon, mandarin,marjorum, scotch spearmint (Mentha cardiaca), mentha longifolio, gardenmint (Mentha spicata), common spearmint (Mentha viridis), orange, andtagetes. (S)-carvone can be extracted from perilla oil and other plantsources including Indian dill, dill, artemisa fergamensis, caraway,Eucalyptus globulus, gingergrass, lavender, Litsea guatemaleusis, andMentha arvensis. Perillyl alcohol, also referred to as perilla alcohol,can be extracted from perilla oil and other plant sources includingAmomum testaceum fruit oil, angelica root oil, bergamot plant, carawayseed oil, gingergrass, lavandin, mandarin oil, orange peel oil, perilla,rose oil otto Bulgaria, savin, turmeric root oil, and wormseed oil.(−)-Myrtenal can also be extracted from other plant sources includingamomum testaceum ridl. fruit oil (Malaysia), Artemisia campestris spp.,Glutoinosa flower oil (Italy), Artemisia variabilis flower oil (Italy),boldo leaf oil (Italy), chamomile oil, cistus oil, coriander seed oil(Cuba), cumin seed, cypress cone oil (Egypt), cypress oil, eucalyptus,eucalyptus globulus pseudoglobulus oil, labdanum leaf oil, labdanum oil,laurel leaf oil (Turkey), layana oil (Kenya), lemon verbena oil(Morocco), mint, nepeta betonicifolia c.a. meyer oil (Turkey), nepetadenudate benth. oil (Iran), parsley leaf oil, pepper, petitgrain sweetoil, peucedanum petriolare boiss oil (Iran), Pteronia oil, SantolinaOil, Satureja viminea l. oil (Costa Rica), Tansy oil (Morocco), wormwoodoil, yarrow leaf oil, and yarrow oil. Perillic acid is also a byproductof limonene metabolism. Limonene is a chiral molecule and is found inbiological sources such as citrus fruits as D-limonene (also referred toas (+)-limonene), which is the (R)-enantiomer. Racemic limonene is knownas dipentene. Perilla oil components and perillaldehyde analogs can beisolated by any means known in the art including, but not limited to,distillation such as steam distillation, cold pressure extraction,chromatography, solvent extraction such as liquid CO₂ extraction ormethanol extraction, or a combination thereof. Perilla oil componentsand perillaldehyde analogs can be chemically synthesized by means knownin the art. Perilla oil components and perillaldehyde analogs can bepurchased from various vendors, for example, Sigma Aldrich (St. Louis,Mo.) or City Chemical (West Haven, Conn.).

In some embodiments, an active agent comprises at least one isolated orsynthesized perilla oil component. Perilla oil components are known inthe art and include, but are not limited to, those set forth in Table A.Perilla oil components include, but are not limited to, farnesene,perillaldehyde, linolenic acid, caryophyllene (includingβ-caryphyollene), limonene (including D-limonene), perillyl alcohol(including (S)-(−)-perillyl alcohol), perillic acid, carvone (including(R)-carvone and (S)-carvone), pinene (including pinene alpha and pinenebeta), linalool, germacrene, bergamotene, and spathulenol.

TABLE A Vapor Solubility Melting Boiling Pressure Viscosity (in waterCAS# Point Point (@ 25° C.) (@ 25° C.) @ 25° C.) Pinene Alpha 80-56-8(−) 62° C. 155.5° C. 4.75 mmHg 2.49 mg/L Pinene Beta 127-91-3 (−) 61° C.166° C. 2.93 mmHg 2.62 mg/L (+)-(R)-Limonene 5989-27-5 (−) 40.8° C. 178°C. 1.541 mmHg 13.8 mg/L Linalool 78-70-6 (−) 11.39° C. 198° C. 0.16 mmHg4.4 mPa 1590 mg/L Perilla Aldehyde 2111-75-3 (−) 4.83° C. 218.2° C.0.0463 mmHg 160.7 mg/L Perillyl Alcohol (racemic) 536-59-4 11.1° C. 244°C. 0.00478 mmHg 471 mg/L Caryophyllene Beta 87-44-5 43.4° C. 256.8° C.0.031 mmHg 0.05 mg/L Caryophyllene Alpha Germacrene D 23986- 15.8° C.262.9° C. 0.023 mmHg 0.013 mg/L 74-5 Bergamotene Trans 13474- 33.7° C.255.4° C. 0.028 mmHg 0.030 mg/L Alpha 59-4 Farnesene Alpha 502-61-4 (−)17.2° C. 261.1° C. 0.025 mmHg 0.011 mg/L Spathulenol 6750-60-3 74.9° C.284.6° C. 1.2 × 10⁻⁴ mmHg 12.4 mg/L Caryophyllene Oxide- 1139-30-6 63°C. 263.5° C. 0.01 mmHg 2.21 mg/L Beta

In some embodiments, an active agent comprises at least one of certainperillaldehyde analogs that have a structure similar to perillaldehydebut differ from perillaldehyde by a single element or group. Inparticular, for the purposes of this specification, perillaldehydeanalogs are limonene (including D-limonene), perillyl alcohol (including(S)-(−)-perillylalcohol), perillic acid (including (S)-(−)-perillicacid), myrtenal (including (1R)-(−)-myrtenal),3-methyl-1-cyclohexene-1-carboxaldehyde, and any other analog ofperillaldehyde that includes substituents on the perillaldehydecyclohexene ring that do not eliminate the ability of the analog to actas a synergist with the insecticides described in this specification.

In some embodiments, an active agent comprises a perillaldehyde analogof Formula (A):

wherein:

R¹ is selected from the group consisting of —CH₂OH, —CHO, and —COOR^(a);

R² is selected from the group consisting of hydrogen, alkyl, andalkenyl;

R³ is selected from the group consisting of hydrogen and alkyl;

R⁴ is hydrogen, or R⁴ and R² are taken together with the atoms to whichthey are attached to form an optionally substituted ring; and

R^(a) is selected from the group consisting of hydrogen and alkyl.

The term “alkyl” refers to a straight or branched saturated hydrocarbonchain. Alkyl groups may include a specified number of carbon atoms. Forexample, C₁-C₁₂ alkyl indicates that the alkyl group may have 1, 2, 3,4, 5, 6, 7, 8, 9, 10, 11, or 12 carbon atoms. An alkyl group may be,e.g., a C₁-C₁₂ alkyl group, a C₁-C₁₀ alkyl group, a C₁-C₈ alkyl group, aC₁-C₆ alkyl group, or a C₁-C₄ alkyl group. For example, exemplary C₁-C₄alkyl groups include methyl, ethyl, n-propyl, isopropyl, n-butyl,sec-butyl, isobutyl and tert-butyl groups. An alkyl group may beoptionally substituted with one or more substituents.

The term “alkenyl” refers to a straight or branched hydrocarbon chainhaving one or more double bonds. Alkenyl groups may include a specifiednumber of carbon atoms. For example, C₂-C₁₂ alkenyl indicates that thealkenyl group may have 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, or 12 carbonatoms. An alkenyl group may be, e.g., a C₂-C₁₂alkenyl group, a C₂-C₁₀alkenyl group, a C₂-C₈ alkenyl group, a C₂-C₆ alkenyl group, or a C₂-C₄alkenyl group. Examples of alkenyl groups include but are not limited toallyl, propenyl, 2-butenyl, 3-hexenyl, and 3-octenyl groups. One of thedouble bond carbons may optionally be the point of attachment of thealkenyl substituent. An alkenyl group may be optionally substituted withone or more substituents.

Substituents may include hydroxy, alkoxy (e.g., methoxy, ethoxy,propoxy, butoxy, and pentoxy), aryloxy groups (e.g., phenoxy,chlorophenoxy, tolyloxy, methoxyphenoxy, benzyloxy,alkyloxycarbonylphenoxy, and acyloxyphenoxy), acyloxy groups (e.g.,propionyloxy, benzoyloxy, and acetoxy), carbamoyloxy groups, carboxygroups, mercapto groups, alkylthio groups, acylthio groups, arylthiogroups (e.g., phenylthio, chlorophenylthio, alkylphenylthio,alkoxyphenylthio, benzylthio, and alkyloxycarbonylphenylthio), halogenatoms, cyano groups, monovalent hydrocarbon groups, substitutedmonovalent hydrocarbon groups, heterogeneous groups, aromatic groups(e.g., phenyl and tolyl), substituted aromatic groups (e.g.,alkoxphenyl, alkoxycarbonylphenyl, and halophenyl), heterocyclic groups,heteroaromatic groups, and amino groups (e.g., amino, mono- anddi-alkylamino having 1 to 3 carbon atoms, methylphenylamino,methylbenzylamino, alkanylamido groups of 1 to 3 carbon atoms,carbamamido, ureido, and guanidino), or any combination thereof.

In some embodiments, an active agent comprises at least one of certaincarvone analogs that have a structure similar to carvone. These analogsretain at least some of the activity of carvone. It is known in the artthat structural modifications can be made to carvone to affect thephysical properties of carvone, such as to reduce its volatility. See,e.g., Olof Smitt, Thesis entitled Syntheses of Allelochemicals forInsect Control (2002), Mid Sweden University, ISSN 1100-7974, ISBN91-7283-277-0, the entire disclosure of which is incorporated into thisspecification by reference. Indeed, the modifications made to thestructure of carvone can in some cases enhance the biological activityof the analog in the composition as compared to carvone. Carvone analogsare shown below in Formulas B-K and include epoxycarvone,hydroxydihydrocarvone, and carvone diols.

In some embodiments, an active agent comprises a synergist which has amodified cyclohexene ring containing a substituted or unsubstitutedmethyl group and other substituents on the ring. Examples of synergistshaving such a modified cyclohexene ring include, but are not limited to,isophorone, 1-methyl-1-cyclohexene, 1-tert-butyl-1-cyclohexene,3,5-dimethyl-2-cyclohexen-1-one, 4-methycyclohexene,7,8-dihydro-α-ionone, 2,4-dimethyl-3-cyclohexenecarboxaldehyde,trivertal, 3-cyclohexene-1-methanol, and terpinolene.

In some embodiments, the insecticide includes, but is not limited to,pyrethrum, pyrethrins, pyrethroids, spinosad, neonicotinoids,sulfoxoflor, carbamates, organophosphates, and organochlorines.

The insecticide can be present in an amount of at least about 0.005%, atleast about 0.01%, at least about 0.05%, at least about 0.1%, at leastabout 0.5%, at least about 1%, at least about 2%, or at least about 3%,at least about 4%, at least about 6%, at least about 8%, at least about10%, at least about 12%, at least about 15%, at least about 20%, atleast about 25%, at least about 30%, at least about 35%, at least about40%, at least about 50% or at least about 55%, at least about 60%, atleast about 65%, at least about 70%, at least about 75%, at least about80%, at least about 85%, at least about 90%, at least about 95%, andless than about 95%, less than about 90%, less than about 80%, less thanabout 75%, less than about 70%, less than about 65%, less than about60%, less than about 55%, less than about 50%, less than about 45%, lessthan about 35%, less than about 30%, less than about 25%, less thanabout 20%, less than about 15%, less than about 10%, less than about 5%,less than about 2.5%, less than about 2%, less than about 1%, less thanabout 0.5%, or less than about 0.1% by weight of the composition.

In some embodiments, the composition comprises an insecticide and activeagent as described in this specification, and is substantially free of,or excludes any amount of, any other insecticide synergist such aspiperonyl butoxide (PBO), N-octyl bicycloheptene dicarboximide(MGK-264), piprotal, propyl isome, sesamex, sesamolin, or sulfoxide. Thecomposition may be substantially free of, or exclude any amount of, oneor more of piperonyl butoxide (PBO), N-octyl bicycloheptenedicarboximide (MGK-264), piprotal, propyl isome, sesamex, sesamolin, orsulfoxide in any combination.

As used in this specification, the term “pyrethrum” refers to a crudeextract composition that is derived from chrysanthemum-like flowersprimarily grown in Kenya, Tanzania, and Australia (e.g., T.cinerariaefolium, C. cinerariaefolium, and C. coccineum) and comprises amixture of the naturally occurring insecticidal ester compounds known asthe “pyrethrins,” as further detailed in U.S. patent application Ser.No. 13/175,405, filed Jul. 1, 2011, which is incorporated into thisspecification by reference in its entirety. “Pyrethrins” is used in thisspecification as a collective term given to any combination of the sixester compounds (including refined pyrethrum) having the general FormulaL and detailed in Table 1.

TABLE 1 (L)

Naturally Occurring Pyrethrin Esters. Common Name CAS Number R₁ R₂Pyrethrins I Jasmolin-I  4466-14-2 CH₃ CH₂CH₃ Cinerin-I 25402-06-6 CH₃CH₃ Pyrethrin-I  121-21-1 CH₃ CH═CH₂ Pyrethrins II Jasmolin-II 1172-63-0 CH₃OC(O) CH₂CH₃ Cinerin-II  121-20-0 CH₃OC(O) CH₃Pyrethrin-II  121-29-9 CH₃OC(O) CH═CH₂

The term “pyrethrin ester” or “pyrethrin” is used in this specificationto refer to one or a combination of two or more of the naturallyoccurring compounds defined in Table 1.

While the terms “pyrethrins” and “pyrethrum” are sometimes usedinterchangeably, “pyrethrum” should be understood here to encompasscrude extracts that contain pyrethrins. The pyrethrins in any givenpyrethrum extract vary in relative amount, depending on factors such asthe plant variety, where it is grown, and the time of harvest.

Because it is not currently commercially advantageous to separate andisolate individual pyrethrin esters from each other, the pyrethrinscontent in pyrethrum extract is typically analyzed for total content ofpyrethrins. While variable, the current state of the art typicallyallows for the total pyrethrins (i.e., pyrethrins I and pyrethrins II)to constitute about 45 to 55% (by weight) of a pyrethrum extract.Besides the pesticidially active esters mentioned above, many plantcomponents may be present in the pyrethrum extract. This extract istypically a high boiling, viscous liquid that is prone to oxidation inair, might be difficult to store for extended periods of time, and canbe readily diluted in a vegetable-based oil carrier to provide aManufacturing Use Product (MUP) containing about 20% pyrethrins. Thisprovides for a longer shelf life and has the added advantage of beingNOSB (National Organic Standards Board) compliant. Therefore, pyrethrinsare approved for use in organic production operations. Pyrethrins arecommercially available from several sources throughout the world and, inthe United States, are available from several sources including theproduct sold under the trade name Pyganic® MUP 20 by MGK (Minneapolis,Minn.). Pyganic® MUP 20 contains about 20% pyrethrins by weight. Whenthe term “MUP 20” is used in this specification it refers to a MUPcomprising about 20% pyrethrins by weight and includes, but is notlimited to, Pyganic® MUP 20.

The term “pyrethroid” is understood in the art to mean one or moresynthetic compounds that act as an insecticide and are adapted from thechemical structure of Formula L. The United States EnvironmentalProtection Agency (EPA) has established two general classes ofpyrethroids. Pyrethroids that include an α-cyano group (C—CN) bonded tothe ester oxygen (see Formula L) are referred to as Type II pyrethroids,while pyrethroids lacking an α-cyano group are referred to as Type Ipyrethroids. See, e.g., EPA Office of Pesticide Programs Memorandum“Pyrethroids: Evaluation of Data from Developmental NeurotoxicityStudies and Consideration of Comparison Sensitivity” (Jan. 20, 2010).Non-limiting examples of pyrethroids include acrinathrin, allethrin,benfluthrin, benzylnorthrin, bioallethrin, bioethanomethrin,bioresmethrin, bifenthrin, cyclethin, cycloprothrin, cyfluthrin,beta-cyfluthrin, gamma-cyhalothrin, lamdba-cyhalothrin, cypermethrin,alpha-cypermethrin, beta-cypermethrin, zeta-cypermethrin, cyphenothrin,deltamethrin, empenthrin, esbiothrin, esfenvalerate, etofenprox,fenfluthrin, fenpropathrin, fenvalerate, flucythrinate, flumethrin,imiprothin, isopyrethrin I, kadethrin, metofluthrin, permethrin, 1RScis-permethrin, phenothrin, prallethrin, resmethrin, silafluofen,sumithrin (d-phenothrin), tau-fluvalinate, tefluthrin, tetramethrin,tralomethrin, transfluthrin, and isomers of these compounds. Etofenprox,a recently registered pyrethroid, contains an ether bond as its centrallinkage rather than an ester bond. In certain embodiments, thepyrethroid comprises at least one of permethrin, sumithrin, prallethrin,resmethrin, etofenprox, allethrin, alpha-cypermethrin, bifenthrinbeta-cypermethrin, cyfluthrin, cypermethrin, deltamethrin,esfenvalerate, etofenprox, lamdba-cyhalothrin, and zeta-cypermethrin,which may be used with, for example, perilla oil, perillaldehyde orcarvone.

Additional information regarding pyrethrum, pyrethrins, and pyrethroidscan be found in various references, reviews, and fact sheets, forexample, Pyrethrum Flowers: Production, Chemistry, Toxicology, and Uses.John E. Casida and Gary B. Quistad (eds.), Oxford University Press,1995; and “Pyrethrins & Pyrethroids” 1998 Fact Sheet published by theNational Pesticide Telecommunications Network (NPTN) at Oregon StateUniversity, Corvallis, Oreg.

Spinosad is an insecticide derived from Saccharopolyspora spinosa. S.spinosa occurs in over 20 natural forms, and over 200 synthetic forms(spinosoids). As used in this specification, spinosad includes at leastone of Spinosyn A, Spinosyn D, or a combination thereof.

Neonicotinoids are insecticides that act on the central nervous systemof insects. Neonicotinoids include, but are not limited to, acetamiprid,clothianidin, dinotefuran, imidacloprid, nitenpyram, thiacloprid, andthiamethoxam.

Carbamates are organic compounds derived from carbamic acid (NH₂COOH)and feature the carbamate ester functional group. Carbamates include,but are not limited to, aldicarb, alanycarb, bendiocarb, benfuracarb,butocarboxim, butoxycarboxim, carbaryl, carbofuran, carbosulfan,ethiofencarb, fenobucarb, formetanate, furathiocarb, isoprocarb,methiocarb, methomyl, metolcarb, oxamyl, pirimicarb, propoxur,thiodicarb, thiofanox, trimethacarb, XMC, xylylcarb, and triazamate.

Organophosphates are esters of phosphoric acid which act on the enzymeacetylcholinesterase. Organophosphates include, but are not limited to,acephate, azamethiphos, azinphos-ethyl, azinphos-methyl, chlorethoxyfos,chlorfenvinphos, chlormephos, chlorpyrifos, methyl chlorpyrifos,coumaphos, cyanophos, demeton-5-methyl, diazinon, dichlorvos/DDVP,dicrotophos, dimethoate, dimethylvinphos, disulfoton, EPN, ethion,ethoprophos, famphur, fenamiphos, fenitrothion, fenthion, flupyrazophos,fosthiazate, heptenophos, isoxathion, malathion, mecarbam,methamidophos, methidathion, mevinphos, monocrotophos, omethoate,oxydemeton-methyl, parathion, methyl parathion, phenthoate, phorate,phosalone, phosmet, phosphamidon, phoxim, pirimiphos-methyl, profenofos,propetamphos, prothiofos, pyraclofos, pyridaphenthion, quinalphos,sulfotep, tebupirimfos, temephos, terbufos, tetrachlorvinphos,thiometon, triazophos, trichlorfon, and vamidothion.

Organochlorines are organic compounds containing at least one covalentlybonded chlorine atom. Organochlorines include, but are not limited to,phthalimides, sulfamides, and chloronitriles, including, but not limitedto, anilazine, captan, chlorothalonil, captafol, chlordane,dichlorodiphenyltrichloroethane (DDT), dicofol, dichlofluanid,dichlorophen, endosulfan, flusulfamide, folpet, hexachlorobenzene,heptachlor, pentachlorphenol and its salts, aldrin, dieldrin, endrin,mirex, phthalide, and tolylfluanid,N-(4-chloro-2-nitro-phenyl)-N-ethyl-4-methyl-benzenesulfonamide.

Compositions

Compositions described in this specification may comprise at least oneactive agent synergist and at least one insecticide. The active agentmay consist of at least one of perilla oil, one of its components, aperillaldehyde or carvone analog, or other related synergist describedin this specification and can be present in an amount of at least about0.01%, at least about 0.1%, at least about 0.5%, at least about 1%, atleast about 2%, or at least about 3%, at least about 4%, at least about6%, or at least about 8%, at least about 10%, at least about 15%, atleast about 20%, at least about 25%, and less than about 99.99%, lessthan about 99.9%, less than about 99%, less than about 95%, less thanabout 90%, less than about 80%, less than about 70%, less than about60%, less than about 50%, less than about 40%, less than about 30%, lessthan about 25%, less than about 20%, less than about 15%, less thanabout 14%, less than about 12%, or less than about 10% by weight of thecomposition. The compositions may comprise at least one of perilla oil,one of its components, a perillaldehyde or carvone analog, or othersynergist described in this specification and may be present in anamount of about 1% to about 15%, about 2% to about 14%, about 6% toabout 12%, or about 8% to about 10% by weight of the composition.Compositions may comprise an active agent that consists of at least oneof perilla oil, one of its components, a perillaldehyde or carvoneanalog, or other synergist described in this specification in an amountof less than about 100%, less than about 99%, less than about 98%, lessthan about 97%, less than about 96%, or less than about 95% by weight ofthe composition. The compositions may comprise an active agent thatconsists of perilla oil, one of its components, a perillaldehyde orcarvone analog, or other synergist described in this specification in anamount of about 1% to about 100%, about 1% to about 99%, about 2% toabout 99%, or about 3% to about 98% by weight of the composition.

For example, in some embodiments, compositions may comprise up to about100% perilla oil. In some embodiments, compositions may comprise 15%perillaldehyde. In some embodiments, compositions may comprise 2%perillaldehyde analog. In some embodiments, compositions may comprise30% perillaldehyde and 30% permethrin.

In addition to a first active agent that consists of perilla oil or oneof its components or a perillaldehyde or carvone analog or othersynergist described in this specification in an amount described above,and depending on the amount of the first active agent, compositions maycomprise a second active agent, such as a different perilla oilcomponent, perillaldehyde or carvone analog, or synergist in the amountsdescribed in the preceding paragraph.

In some embodiments, compositions may comprise at least one insecticideselected from the group consisting of pyrethrum, pyrethrins,pyrethroids, spinosad, neonicotinoids, sulfoxoflor, carbamates,organophosphates, and organochlorines. The insecticide can be present inan amount of at least about 1%, at least about 2%, at least about 4%, atleast about 6%, or at least about 8%, less than about 15%, less thanabout 14%, less than about 12%, or less than about 10% by weight of thecomposition. The compositions may comprise an insecticide in an amountof about 1% to about 15%, about 2% to about 14%, about 6% to about 12%,or about 8% to about 10% by weight of the composition.

In addition to a first active agent that consists of perilla oil or oneof its components or a perillaldehyde or carvone analog or othersynergist described in this specification in an amount described above,at least one insecticide, such as at least one selected from the groupconsisting of pyrethrum, pyrethrins, pyrethroids, spinosad,neonicotinoids, sulfoxoflor carbamates, organophosphates, andorganochlorines in an amount described above, and an optional secondactive agent comprising a different perilla oil component, depending onthe amount of the first and second active agents, compositions maycomprise a third active agent consisting of a different perilla oilcomponent or a different insecticide selected from the group consistingof pyrethrum, pyrethrins, pyrethroids, spinosad, neonicotinoids,sulfoxoflor, carbamates, organophosphates, and organochlorines in anamount of at least about 1%, at least about 2%, at least about 4%, atleast about 6%, or at least about 8%, less than about 15%, less thanabout 14%, less than about 12%, less than about 10% by weight of thecomposition. The compositions may comprise a third active agent in anamount of at least about 1%, at least about 2%, at least about 3%, atleast about 4%, at least about 5%, at least about 6%, at least about 7%,at least about 8%, at least about 9%, or at least about 10%, and lessthan about 99.9%, less than about 99%, less than about 95%, less thanabout 75%, less than about 50%, less than about 40%, less than about35%, less than about 25%, less than about 20%, less than about 15%, lessthan about 14%, less than about 12%, or less than about 10% by weight ofthe composition. The compositions may comprise a third active agent thatconsists of perilla oil or one of its components in an amount of about1% to about 100%, about 1% to about 99%, about 2% to about 99%, or about3% to about 98% by weight of the composition.

Compositions may further comprise a viscosity modifier such as one ormore of mineral oil or glycerol. “Mineral oil” as used in thisspecification relates to the commonly known product of the same name,which is a by-product of the distillation of petroleum (crude oil) tomake gasoline and other products. Mineral oil is typically transparentand colorless and comprises complex mixtures of long chain aliphaticcompounds often ranging in size from C₁₅-C₄₀. Depending on the refiningprocess and source of crude oil, mineral oils can also includeparaffinic, naphthenic, and aromatic compounds in varying weightpercentages. Synonymous names for mineral oil can include “paraffin oil”or “white mineral oil” among other common names. Mineral oil isavailable from any number of commercial distributors (e.g., Brenntag,ProChem, Inc.). Non-limiting examples of “mineral oil” include thoseidentified by CAS registry numbers: 8012-95-1, 8020-83-5, 8042-47-5,72623-84-8, 72623-86-0, 72623-87-1, 64741-88-4, 64741-89-5, 64742-54-7,64742-55-8, 64742-56-9, and 64742-65-0. The compositions may comprise aviscosity modifier, such as mineral oil glycerol, or any combination ofviscosity modifiers, in an amount of at least about 10%, at least about15%, at least about 20%, at least about 25%, at least about 30%, atleast about 35%, at least about 40%, at least about 45%, at least about50%, at least about 55%, at least about 60%, at least about 65%, or atleast about 70% by weight of the composition. The compositions maycomprise a viscosity modifier, such as mineral oil, glycerol, or anycombination of viscosity modifiers, in an amount of less than about 99%,less than about 95%, less than about 90%, less than about 85%, or lessthan about 80% by weight of the composition. The compositions maycomprise a viscosity modifier, such as mineral oil, glycerol, or acombination of viscosity modifiers, in an amount of about 10% to about99%, about 15% to about 99%, about 20% to about 99%, about 25% to about99%, about 30% to about 99%, about 35% to about 99%, about 40% to about99%, about 45% to about 99%, about 50% to about 99%, about 55% to about99%, about 60% to about 99%, about 65% to about 99%, about 70% to about99%, about 70% to about 95%, about 70% to about 90%, about 60% to about90%, about 50% to about 90%, about 40% to about 90%, about 30% to about90%, about 20% to about 90%, about 10% to about 90%, about 70% to about85%, or about 70% to about 80% by weight of the composition.

In some embodiments, a composition can include one or more carriersand/or diluents such as, for example, any solid or liquid carrier ordiluent that is commonly used in pesticidal, agricultural, orhorticultural compositions. Suitably, any included additional carrier ordiluent will not reduce the insecticidal efficacy of the composition,relative to the efficacy of the composition in the absence of theadditional component. Carriers and diluents can include, for example,solvents (e.g., water, alcohols, petroleum distillates, acids, andesters); vegetable (including, but not limited to, methylated vegetable)and/or plant-based oils as well as ester derivatives thereof (e.g.,wintergreen oil, cedarwood oil, rosemary oil, peppermint oil, geraniol,rose oil, palmarosa oil, citronella oil, citrus oils (e.g., lemon, lime,and orange), dillweed oil, corn oil, sesame oil, soybean oil, palm oil,vegetable oil, olive oil, peanut oil, and canola oil). The compositioncan include varying amounts of other components such as, for example,surfactants (e.g., non-ionic, anionic, cationic, and zwitterionicsurfactants); fatty acids and fatty acid esters of plant oils (e.g.,methyl palmitate/oleate/linoleate); and other auxiliary ingredients suchas, for example, emulsifiers, dispersants, stabilizers, suspendingagents, penetrants, coloring agents/dyes, UV-absorbing agents, andfragrances, as necessary or desired. The compositions may comprisecarrier or diluent in an amount of at least about 5% or at least about10% by weight of the composition. The compositions may comprise carrieror diluent in an amount of less than about 90% or less than about 80% byweight of the composition. The compositions may comprise carrier ordiluent in an amount of about 5% to about 90%, or about 10% to about 80%by weight of the composition. Components other than active agent(s) canbe included in the compositions in any amount as long as the compositionhas some amount of insecticidal efficacy.

Components of a composition can have a synergistic or additive effect oninsecticidal activity. Components have an additive effect when theeffect of the combination is equal to the sum of the effects of eachindividual component. In contrast, components have a synergistic effectwhen the effect of the combination exceeds the sum of the effects of thecomponents when applied individually. The effect (E) of a combination oftwo compounds may be calculated using the Colby formula (1) (S. R.Colby, “Calculating Synergistic and Antagonistic Responses of HerbicideCombinations”, Weeds 1967, 15, 20-22):

$\begin{matrix}{E = {X + Y - \frac{X \times Y}{100}}} & (1)\end{matrix}$

wherein X is the kill rate, expressed as a percentage of the untreatedcontrol, when employing active compound X′ at an application rate of mg/ha or in a concentration of m ppm, μg, or other appropriate unit;wherein Y is the kill rate, expressed as a percentage of the untreatedcontrol, when employing active compound Y′ at an application rate of ng/ha or in a concentration of n ppm, μg, or other appropriate unit;wherein E is the kill rate, expressed as a percentage of the untreatedcontrol, when employing active compounds X′ and Y′ at application ratesof m and n g/ha or in a concentration of m and n ppm. If the actualinsecticidal kill rate is the calculated value (E), then the action ofthe combination is additive. If the actual insecticidal kill rateexceeds the calculated value (E), then the action of the combination issuper-additive, that is, a synergistic effect is present. If theinsecticidal kill rate is lower than the calculated value (E), then theaction of the combination is considered antagonistic.

As shown in the Examples, perilla oil and some of its components, aperillaldehyde or carvone analog, or other synergist can havesynergistic activity with insecticides such as pyrethrum, pyrethrins,pyrethroids, spinosad, neonicotinoids, sulfoxoflor, carbamates,organophosphates, and organochlorines. The nature of the synergisticactivity is unknown; however, without being limited to theory, it ispostulated that perilla oil, its components or a perillaldehyde orcarvone analog or other related synergist may be preventing thedegradation of insecticides by blocking detoxifying enzymes such as theoxidases (P450's), esterases (COE's), and transferases (GST's), all ofwhich have been implicated in rendering exogenous toxins such asinsecticides inactive.

As an example, compositions may comprise a perilla oil component, suchas carvone, or a perillaldehyde or carvone analog, and an insecticide,such as a neonicotinoid, wherein the perilla oil component orperillaldehyde or carvone analog acts as a synergist to increase theefficacy or activity of the insecticide. The perilla oil component maybe present in the composition with the insecticide.

Embodiments include commercially useful formulations or “ready-to-use”application forms. In such formulations, the composition can be suitablyprovided as a mixture with other active compounds, for example, variousadditional insecticides, pesticides, fungicides, anti-microbials, and/orherbicides, as well as plant growth regulators, insect repellents,attractants, fertilizers, and/or fragrances, to expand the applicabilityof the insecticidal composition described in this specification.Embodiments provide for the compositions manufactured as formulationsthat are useful for insect control. In some embodiments, the compositioncan be formulated as an emulsion, a liquid concentrate, a sol (flowableagent), an aerosol (e.g., fogger), a liquid for ultra low volume (ULV)application, a mist, a spray, a vapor, a surface contact treatment, orincorporated into fibers or other materials such as a bednet, or thelike, by any standard or conventional methods for mixing andmanufacturing such formulations such as, for example, admixing activeagent and an amount of mineral oil, glycerol, other viscosity modifier,or combination thereof, and optionally with one or more of any suitableadditional inert ingredient that is used as a carrier, solvent, diluent,emulsifier, dispersant, stabilizers, suspending agent, or penetrant. Theaddition of these materials would depend on the active ingredient andthe type of formulation and how it is intended to be applied.Compositions suitable for a particular application type can beformulated by those of skill in the art based on standard andconventional methods using guidance provided in this specification.

In some embodiments, the composition can be formulated for applicationor delivery as an aerosol or a fog wherein the composition allows forthe formation of droplets having an average diameter of about 1 μm toabout 30 μm. Suitable compositions for such a formulation typicallyshould have a viscosity that allows for the composition to atomize, butnot be so thick as to clog the nozzle. Such viscosities can vary and bereadily determined by one of skill in the art; however, a non-limitingcommon minimum viscosity is about 70 centistokes (cts).

Plants or plant cells that have been modified to produce a perilla oilcomponent, perillaldehyde or carvone analog, or synergist described inthis specification are also provided. In certain embodiments, the plantsor plant cells are modified to contain or express polynucleotides and/orpolypeptides that facilitate the synthesis of, or increase the synthesisof, a perilla oil component or perillaldehyde analog or synergist in theplant. In certain embodiments, the plants are further modified toproduce a pesticide in the plant, in addition to a perilla oilcomponent, perillaldehyde analog, or combination thereof. In certainembodiments, the modified plants exhibit enhanced or increasedresistance to insect or pest attack when compared with control plants orplant cells. In certain embodiments, the modified plants or plant cellsexhibit enhanced growth, yield or a combination thereof relative tocontrol plants. Modified plants may include vegetable, herb, spice, orfruit crops, as well as plants or crops producing cotton, flax, tobacco,hemp, rubber, nuts, and nursery stock and ornamental plant parts.Modified plants may include crops such as soybeans, corn, canola,oilseed rape, cotton, sugar beet, alfalfa, peanuts, wheat, barley, rye,oats, millet, and rice.

Transgenic plants and methods of producing transgenic plants areprovided. Such transgenic plants are produced, in certain embodiments,by introducing into a plant or plant cell one or more polynucleotidesencoding one or more polypeptides that are involved in the synthesis ofa perilla oil component or perillaldehyde analog, such that thepolynucleotide is heterologously expressed and the perilla oil componentor perillaldehyde analog is produced. In certain embodiments, expressionof such polynucleotides or polypeptides may be down regulated, forexample, by antisense, RNAi, micro RNAs, or sense suppression. Incertain embodiments, the polynucleotide is provided as a construct inwhich a promoter is operably linked to the polynucleotide. The synthesispathways and enzymes responsible for producing many perilla oilcomponents and perillaldehyde analogs are known to those of skill in theart. For example, the isoprenyl synthesis pathway is well understood.Polypeptide enzymes that may be modified include, but are not limitedto, monoterpene synthase, limonene-6-hydroxylase, (+)-trans-carveoldehydrogenase, mevalonate kinases, acetoacetyl-CoA thiolase, 3-hydroxy3-methylgluteryl-CoA transferase, prenyl transferases, terpenesynthases, transketolases. One of skill in the art would understand howto manipulate de novo, enhanced or reduced expression and activity ofsuch polypeptides, such that production of a perilla oil component orperillaldehyde analog is effected, increased or decreased in the plant.Accordingly, the transgenic plant can be modified to express one or moreof farnesene, perillaldehyde, linolenic acid, caryophyllene, limonene,carvone, perillyl alcohol, pinene, linalool, germacrene, bergamotene,and spathulenol wherein the active agent has a synergistic effect oninsecticidal activity. In certain embodiments, methods for controllinginsect pests on a transgenic plant are provided in which a transgenicplant expressing a perilla oil component or perillaldehyde analog iscontacted with an insecticide using one or more methods of applicationdescribed in this specification for the compositions of the invention.The perilla oil component or perillaldehyde analog is expressed in theplant in an amount effective to have a synergistic effect on theinsecticide.

As used in this specification, a “control plant” is a plant that issubstantially equivalent to a test plant or modified plant in allparameters with the exception of the test parameters. For example, whenreferring to a plant into which a polynucleotide encoding a polypeptideinvolved in the synthesis of a perilla oil component or perillaldehydeanalog, in certain embodiments, a control plant is an equivalent plantinto which either no such polynucleotide has been introduced. In certainembodiments, a control plant is an equivalent plant into which a controlpolynucleotide has been introduced. In such instances, the controlpolynucleotide is one that is expected to result in little or nophenotypic effect on the plant.

The polynucleotides encoding polypeptides involved in the synthesis of aperilla oil component or perillaldehyde analog may be introduced into aplant cell to produce a transgenic plant. As used in this specification,“introduced into a plant” with respect to polynucleotides encompassesthe delivery of a polynucleotide into a plant, plant tissue, or plantcell using any suitable polynucleotide delivery method. Methods suitablefor introducing polynucleotides into a plant useful in the practice ofthe present invention include, but are not limited to, freeze-thawmethod, microparticle bombardment, direct DNA uptake, whisker-mediatedtransformation, electroporation, sonication, microinjection, plantvirus-mediated, and Agrobacterium-mediated transfer to the plant. Anysuitable Agrobacterium strain, vector, or vector system for transformingthe plant may be employed according to the present invention.

In some embodiments, a plant may be regenerated or grown from the plant,plant tissue or plant cell. Any suitable methods for regenerating orgrowing a plant from a plant cell or plant tissue can be used, such as,without limitation, tissue culture or regeneration from protoplasts.Plants may be regenerated by growing transformed plant cells on callusinduction media, shoot induction media and/or root induction media.

The polynucleotides to be introduced into the plant can be operablylinked to a promoter sequence and can be provided as a construct. Asused in this specification, a polynucleotide is “operably linked” whenit is placed into a functional relationship with a second polynucleotidesequence. For instance, a promoter is operably linked to a codingsequence if the promoter is connected to the coding sequence such thatit may effect transcription of the coding sequence. In variousembodiments, the polynucleotides may be operably linked to at least one,at least two, at least three, at least four, at least five, or at leastten promoters.

Promoters useful in the practice of the present invention include, butare not limited to, constitutive, inducible, temporally-regulated,developmentally regulated, chemically regulated, tissue-preferred andtissue-specific promoters. Suitably, the promoter causes sufficientexpression in the plant to produce the phenotypes described in thisspecification. Suitable promoters include, but are not limited to, the35S promoter of the cauliflower mosaic virus, ubiquitine, tCUP crypticconstitutive promoter, the Rsyn7 promoter, pathogen-inducible promoters,the maize In2-2 promoter, the tobacco PR-1a promoter,glucocorticoid-inducible promoters, and tetracycline-inducible andtetracycline-repressible promoters.

The modified plant producing the perilla oil component or perillaldehydeanalog component may have a composition comprising an insecticide, asdescribed in this specification, applied such that the insecticidecontacts the plant. Upon application of the insecticide, the perilla oilcomponent is expressed or produced by the plant in an amount effectiveto act as a synergist to increase the efficacy or activity of theinsecticide against an insect pest, such as those described in thisspecification. In plants modified to produce a pesticide and a perillaoil component or perillaldehyde, enhanced resistance to insect pestsdescribed in this specification may be achieved without application of apesticide.

Methods for Making Compositions

The compositions can be generally prepared by any appropriatemanufacturing processes and using any appropriate manufacturingequipment such as is known in the art. Suitably, the compositions can beprepared by combining the various components in an appropriate vessel(considering vessel size, amount of composition to be made andreactivity of components) with mixing (e.g., stirring) until a uniformor homogeneous composition is achieved. The various compositioncomponents can be added sequentially, with stirring between eachaddition to ensure dissolution and/or dispersion of the previouscomponent. This may be followed by addition of one or more additionalcomponents (e.g., solvents, diluents, and carriers) with stirring toprovide a homogeneous composition.

Methods

In some aspects, the disclosure provides methods for insect controlcomprising contacting an insect with an amount of any of thecompositions described in this specification. As used in thisspecification, insects may include, but are not limited to, mosquitoes.“Mosquito” is understood to refer to any species of the approximately3,500 species of the insect that is commonly associated with and giventhe common name, “mosquito.” Mosquitoes span 41 insect genera, includingthe non-limiting examples of Aedes, Culex, Anopheles (carrier ofmalaria), Coquillettidia, and Ochlerotatus. In embodiments described inthis specification, a mosquito can refer to an adult mosquito or alarval mosquito or both. Thus, some embodiments describe methods orcompositions wherein the insecticidal activity is referred to asmosquito “adulticide” or alternatively a mosquito “larvacide.” Insectsmay further include agronomic pests including, but not limited to,insects of the orders Lepidoptera (moths), Coleoptera (beetles), andHemiptera (sucking insects, true bugs). Contacting an insect with acomposition includes, but is not limited to, exposing an insect or apopulation of insects either by direct contact using any methoddescribed in this specification or known in the art, such as by topicalapplication, or by indirect contact such as by inhalation of a vapor,spray, mist, aerosol or fog or by ingestion of the composition by theinsect.

Perilla oil, the perilla oil components, the perillaldehyde and carvoneanalogs, and the synergists having a cyclohexene ring described in thisspecification also have a synergistic effect with insecticides, such aspyrethrum, pyrethrins, pyrethroids, neonicotinoids, carbamates,organophosphates and organochlorines when used to control agronomonicpests. Agronomic pests include larvae of the order Lepidoptera, such asarmyworms, (e.g., beet armyworm (Spodoptera exigua)), cutworms, loopers,(e.g., cabbage looper (Trichoplusia ni)) and heliothines in the familyNoctuidae (e.g., fall armyworm (Spodoptera fugiperda J. E. Smith), beetarmyworm (Spodoptera exigua Hubner), black cutworm (Agrotis ipsilonHufnagel), and tobacco budworm (Heliothis virescens Fabricius)); borers,casebearers, webworms, coneworms, cabbageworms and skeletonizers fromthe family Pyralidae (e.g., European corn borer (Ostrinia nubilalisHubner), navel orangeworm (Amyelois transitella Walker), corn rootwebworm (Crambus caliginosellus Clemens), and sod webworms (Pyralidae:Crambinae) such as sod webworm (Herpetogramma licarsisalis Walker));leafrollers, budworms, seed worms, and fruit worms in the familyTortricidae (e.g., codling moth (Cydia pomonella Linnaeus), grape berrymoth (Endopiza viteana Clemens), and oriental fruit moth (Grapholitamolesta Busck)); and many other economically important Lepidoptera(e.g., diamondback moth (Plutella xylostella Linnaeus), pink bollworm(Pectinophora gossypiella Saunders), silverleaf whitefly (Bemisiaargentifolii), and gypsy moth (Lymantria dispar Linnaeus)); foliarfeeding larvae and adults of the order Coleoptera including weevils fromthe families Anthribidae, Bruchidae, and Curculionidae (e.g., bollweevil (Anthonomus grandis Boheman), rice water weevil (Lissorhoptrusoryzophilus Kuschel), granary weevil (Sitophilus granarius Linnaeus),rice weevil (Sitophilus oryzae Linnaeus), annual bluegrass weevil(Listronotus maculicollis Dietz), bluegrass billbug (Sphenophorusparvulus Gyllenhal), hunting billbug (Sphenophorus venatus vestitus),and Denver billbug (Sphenophorus cicatristriatus Fahraeus)); fleabeetles, cucumber beetles, rootworms, leaf beetles, potato beetles, andleafminers in the family Chrysomelidae (e.g., Colorado potato beetle(Leptinotarsa decemlineata Say)); western corn rootworm (Diabroticavirgifera virgifera LeConte); western flower thrip (Frankliniellaoccidentalis)); chafers and other beetles from the family Scaribaeidae(e.g., Japanese beetle (Popillia japonica Newman), oriental beetle(Anomala orientalis Waterhouse), northern masked chafer (Cyclocephalaborealis Arrow), southern masked chafer (Cyclocephala immaculateOlivier), black turfgrass ataenius (Ataenius spretulus Haldeman), greenJune beetle (Cotinis nitida Linnaeus), Asiatic garden beetle (Maladeracastanea Arrow), May/June beetles (Phyllophaga spp.) and European chafer(Rhizotrogus majalis Razoumowsky)); carpet beetles from the familyDermestidae; wireworms from the family Elateridae; bark beetles from thefamily Scolytidae; flour beetles from the family Tenebrionidae;leafhoppers (e.g., Empoasca spp.) from the family Cicadellidae;planthoppers from the families Fulgoroidae and Delphacidae (e.g., cornplant hopper (Peregrinus maidis)); treehoppers from the familyMembracidae; psyllids from the family Psyllidae; whiteflies from thefamily Aleyrodidae; aphids from the family Aphididae, such as Aphisgossypii (cotton melon aphid), Acyrthisiphon pisum Harris (pea aphid),Aphis craccivora Koch (cowpea aphid), Aphis fabae Scopoli (black beanaphid), Aphis gossypii Glover (cotton aphid, melon aphid), Aphis pomi DeGeer (apple aphid), Aphis spiraecola Patch (spirea aphid), Aulacorthumsolani Kaltenbach (foxglove aphid), Chaetosiphon fragaefolii Cockerell(strawberry aphid), Diuraphis noxia Kurdjumov/Mordvilko (Russian wheataphid), Dysaphis plantaginea Paaserini (rosy apple aphid), Eriosomalanigerum Hausmann (woolly apple aphid), Hyalopterus pruni Geoffroy(mealy plum aphid), Lipaphis erysimi Kaltenbach (turnip aphid),Metopolophium dirrhodum Walker (cereal aphid), Macrosipum euphorbiaeThomas (potato aphid), Myzus persicae Sulzer (peach-potato aphid, greenpeach aphid), Nasonovia ribisnigri Mosley (lettuce aphid), Pemphigusspp. (root aphids and gall aphids), Rhopalosiphum maidis Fitch (cornleaf aphid), Rhopalosiphum padi Linnaeus (bird cherry-oat aphid),Schizaphis graminum Rondani (greenbug), Sitobion avenae Fabricius(English grain aphid), Therioaphis maculata Buckton (spotted alfalfaaphid), Toxoptera aurantii Boyer de Fonscolombe (black citrus aphid),Toxoptera citricida Kirkaldy (brown citrus aphid) and green peach aphid(Myzus persicae); phylloxera from the family Phylloxeridae; mealybugsfrom the family Pseudococcidae; scales from the families Coccidae,Diaspididae, and Margarodidae; lace bugs from the family Tingidae; stinkbugs from the family Pentatomidae; flat mites in the familyTenuipalpidae (e.g., citrus flat mite (Brevipalpus lewisi McGregor));rust and bud mites in the family Eriophyidae and other foliar feedingmites; chinch bugs (e.g., hairy chinch bug (Blissus leucopterus hirtusMontandon) and southern chinch bug (Blissus insularis Barber) and otherseed bugs from the family Lygaeidae); spittlebugs from the familyCercopidae; squash bugs from the family Coreidae; red bugs and cottonstainers from the family Pyrrhocoridae; and adults and immatures of theorder Orthoptera including grasshoppers, locusts, and crickets (e.g.,migratory grasshoppers (e.g., Melanoplus sanguinipes Fabricius, M.differentialis Thomas)), American grasshoppers (e.g., Schistocercaamericana Drury), desert locust (Schistocerca gregaria Forskal),migratory locust (Locusta migratoria Linnaeus), bush locust (Zonocerusspp.); adults and immatures of the order Diptera including leafminers,midges, fruit flies (Tephritidae), frit flies (e.g., Oscinella fritLinnaeus), soil maggots, adults and nymphs of the orders Hemiptera andHomoptera such as plant bugs from the family Miridae; adults andimmatures of the order Thysanoptera including onion thrips (Thripstabaci Lindeman), flower thrips (Frankliniella spp.), and other foliarfeeding thrips; and cicadas from the family Cicadidae. Agronomic pestsalso include Classes Nematoda, Cestoda, Trematoda, and Acanthocephalaincluding economically important members of the orders Strongylida,Ascaridida, Oxyurida, Rhabditida, Spirurida, and Enoplida such aseconomically important agricultural pests (e.g., root knot nematodes inthe genus Meloidogyne, lesion nematodes in the genus Pratylenchus, andstubby root nematodes in the genus Trichodorus).

Perilla oil, the perilla oil components, the perillaldehyde and carvoneanalogs, and the synergists having a cyclohexene ring described in thisspecification also have a synergistic effect with insecticides, such aspyrethrum, pyrethrins, pyrethroids, neonicotinoids, carbamates,organophosphates and organochlorines when used to control agronomonicpests. Agronomic and non-agronomic pests include nymphs and adults ofthe order Blattodea including cockroaches from the families Blattellidaeand Blattidae (e.g., oriental cockroach (Blatta orientalis Linnaeus),Asian cockroach (Blatella asahinai Mizukubo), German cockroach(Blattella germanica Linnaeus), brownbanded cockroach (Supellalongipalpa Fabricius), American cockroach (Periplaneta americanaLinnaeus), brown cockroach (Periplaneta brunnea Burmeister), Madeiracockroach (Leucophaea maderae Fiabricius), smoky brown cockroach(Periplaneta fuliginosa Service), Australian Cockroach (Periplanetaaustralasiae Fabr.), lobster cockroach (Nauphoeta cinerea Olivier) andsmooth cockroach (Symploce pallens Stephens)); adults and larvae of theorder Dermaptera including earwigs from the family Forficulidae (e.g.,European earwig (Forficula auricularia Linnaeus), and black earwig(Chelisoches morio Fabricius)). Also included are adults and larvae ofthe order Acari (mites) such as spider mites and red mites in the familyTetranychidae (e.g., European red mite (Panonychus ulmi Koch), twospotted spider mite (Tetranychus urticae Koch), and McDaniel mite(Tetranychus mcdanieli McGregor)); mites important in human and animalhealth (e.g., dust mites in the family Epidermoptidae, follicle mites inthe family Demodicidae, and grain mites in the family Glycyphagidae);ticks in the order Ixodidae (e.g., deer tick (Ixodes scapularis Say),Australian paralysis tick (Ixodes holocyclus Neumann), American dog tick(Dermacentor variabilis Say), and lone star tick (Amblyomma americanumLinnaeus)); scab and itch mites in the families Psoroptidae, Pyemotidae,and Sarcoptidae; crickets such as house cricket (Acheta domesticusLinnaeus), mole crickets (e.g., tawny mole cricket (Scapteriscus vicinusScudder), and southern mole cricket (Scapteriscus borellii Giglio-Tos));flies including house flies (e.g., Musca domestica Linnaeus), lesserhouse flies (e.g., Fannia canicularis Linnaeus, F. femoralis Stein),stable flies (e.g., Stomoxys calcitrans Linnaeus), face flies, hornflies, blow flies (e.g., Chrysomya spp., Phormia spp.), and othermuscoid fly pests, horse flies (e.g., Tabanus spp.), bot flies (e.g.,Gastrophilus spp., Oestrus spp.), cattle grubs (e.g., Hypoderma spp.),deer flies (e.g., Chrysops spp.), keds (e.g., Melophagus ovinusLinnaeus) and other Brachycera; mosquitoes (e.g., Aedes spp., Anophelesspp., Culex spp.), black flies (e.g., Prosimulium spp., Simulium spp.),biting midges, sand flies, sciarids, and other Nematocera; insect pestsof the order Hymenoptera including ants (e.g., red carpenter ant(Camponotus ferrugineus Fabricius), black carpenter ant (Camponotuspennsylvanicus De Geer), Pharaoh ant (Monomorium pharaonis Linnaeus),little fire ant (Wasmannia auropunctata Roger), fire ant (Solenopsisgeminata Fabricius), red imported fire ant (Solenopsis invicta Buren),Argentine ant (Iridomyrmex humilis Mayr), crazy ant (Paratrechinalongicomis Latreille), pavement ant (Tetramorium caespitum Linnaeus),cornfield ant (Lasius alienus Forster), odorous house ant (Tapinomasessile Say)); insect pests of the Family Formicidae including theFlorida carpenter ant (Camponotus floridanus Buckley), white-footed ant(Technomyrmex albipes fr. Smith), big headed ants (Pheidole spp.), andghost ant (Tapinoma melanocephalum Fabricius); bees (including carpenterbees), hornets, yellow jackets, wasps, and sawflies (Neodiprion spp.;Cephus spp.); insect pests of the order Isoptera including termites inthe Termitidae (ex. Macrotermes sp.), Kalotermitidae (ex. Cryptotermessp.), and Rhinotermitidae (ex. Reticulitermes spp., Coptotermes spp.),families the eastern subterranean termite (Reticulitermes flavipesKollar), western subterranean termite (Reticulitermes hesperus Banks),Formosan subterranean termite (Coptotermes formosanus Shiraki), WestIndian drywood termite (Incisitermes immigrans Snyder), powder posttermite (Cryptotermes brevis Walker), drywood termite (Incisitermessnyderi Light), southeastern subterranean termite (Reticulitermesvirginicus Banks), western drywood termite (Incisitermes minor Hagen),arboreal termites such as Nasutitermes sp. and other termites ofeconomic importance; insect pests of the order Thysanura such assilverfish (Lepisma saccharina Linnaeus) and firebrat (Thermobiadomestica Packard); insect pests of the order Mallophaga and includingthe head louse (Pediculus humanus capitis De Geer), body louse(Pediculus humanus humanus Linnaeus), chicken body louse (Menacanthusstramineus Nitszch), dog biting louse (Trichodectes canis De Geer),fluff louse (Goniocotes gallinae De Geer), sheep body louse (Bovicolaovis Schrank), short-nosed cattle louse (Haematopinus eurysternusNitzsch); long-nosed cattle louse (Linognathus vituli Linnaeus) andother sucking and chewing parasitic lice that attack man and animals;insect pests of the order Siphonoptera including the oriental rat flea(Xenopsylla cheopis Rothschild), cat flea (Ctenocephalides felisBouche), dog flea (Ctenocephalides canis Curtis), hen flea(Ceratophyllus gallinae Schrank), sticktight flea (Echidnophagagallinacea Westwood), human flea (Pulex irritans Linnaeus) and otherfleas afflicting mammals and birds. Arthropod pests also include spidersin the order Araneae such as the brown recluse spider (Loxoscelesreclusa Gertsch & Mulaik) and the black widow spider (Latrodectusmactans Fabricius), and centipedes in the order Scutigeromorpha such asthe house centipede (Scutigera coleoptrata Linnaeus).

In some embodiments, the method comprises contacting an insect with anamount of any of the compositions described in this specificationeffective to control at least about 20%, at least about 30%, at leastabout 40%, at least about 50%, less than about 100%, less than about90%, less than about 80%, less than about 70%, or less than about 60% ofthe contacted adult insect population. In some embodiments, the methodcomprises contacting an insect with an amount of any of the compositionsdescribed here effective to provide about 95% insect mortality. In someembodiments, the compositions provided in this specification comprise anamount (e.g., weight %) of at least one active agent that is suitably ina range that allows for at least some degree of insecticidal efficacy(e.g., more than 0%, but less that 95% insect mortality rate) when thecomposition is used, while not necessarily meeting the EPA requirementsfor a registered insecticide. For a composition to be registered andmarketed as a “pesticide” within the United States for some uses (e.g.,public health uses and pest control in residential structures) the EPArequires that a composition exhibits a 95% insect mortality at thelowest labeled rate. The EPA also regulates the upper limits of activeagent(s) that can be used in practice in the environment.

In some embodiments, methods for insect control or controlling insectscomprise contacting an insect with an amount of any of the compositionsdescribed in this specification. Control or controlling includeskilling, knocking down, or a combination thereof, of at least a portionof a population of insects. A population includes at least two insects.Insect knockdown does not necessarily correlate to insect death, asinsects can recover after the initial knockdown. In some embodiments,the composition is applied in an amount effective to knockdown at leastabout 20%, at least about 30%, at least about 40%, at least about 50%,at least about 60%, at least about 70%, at least about 80%, at leastabout 90%, at least about 95%, or at least about 98% of the contactedinsect population. In some embodiments, the composition is applied in anamount effective to kill at least about 20%, at least about 30%, atleast about 40%, at least about 50%, at least about 60%, at least about70%, at least about 80%, at least about 90%, at least about 95%, or atleast about 98% of the contacted insect population.

In some embodiments, the methods described here can comprise any knownroute, apparatus, and/or mechanism for the delivery or application ofthe compositions and formulations. In some embodiments, compositions maybe applied as an aerosol, mist, fog, vapor, or ULV spray. In someembodiments, compositions may be applied as a surface contact treatment.A surface contact treatment includes surfaces that have been contactedwith the composition, such as by painting, rolling, coating, dip coatingor spraying the surface, or the compositions may be incorporated intofibers or other materials, such as, for example, a bednet to produce amaterial comprising a surface contact treatment. In some embodiments,the method comprises a sprayer. Traditional pesticide sprayers in thepest control markets are typically operated manually or electrically orare gas-controlled and use maximum pressures ranging from 15 to 500 psigenerating flow rates from 5 gpm to 40 gpm. In other embodiments, themethods disclosed here comprise the use of the compositions and/orformulations in combination with any low volume environmental pestcontrol device(s) such as, for example, ultra low volume (ULV) machines.Such combinations are useful in methods for mosquito control as well asother flying insects (e.g., flies, gnats, and flying ants) whereincontacting the insect with a low volume of the composition is possibleand/or desirable. ULV machines suitably use low volume of material, forexample at rates of about one gallon per hour (or ounces per minute),and typically utilize artificial wind velocities such as from, forexample, an air source (e.g., pump or compressor) to break down anddistribute the composition/formulation into a cold fog (suitably havingaverage droplet particle sizes of about 1-30 μm). Any standard groundULV equipment used for insect control such as, for example, a systemincluding a (CETI) Grizzly aerosol generator can be used in the methodsdescribed here. A general ULV system includes a tank for the composition(e.g., insecticide), a transport system (e.g., a pump or pressurizedtank), a flow control device, and a nozzle that atomizes thecomposition. Typically, ULV machines do not compress droplets. Rather,they often use a venture siphoning system, and can induce an artificialenergizing of the droplets by adding an electrical current to the liquid(e.g., through the use an electrode located at the application tip). SeeU.S. Pat. No. 3,516,608 (Bowen et al.) incorporated here by reference.

It is to be understood that any numerical range recited in thisspecification includes all values from the lower value to the uppervalue. For example, if a concentration range is stated as 1% to 50%, itis intended that values such as 2% to 40%, 10% to 30%, or 1% to 3%,etc., are expressly enumerated in this specification. It is also to beunderstood that any numerical range recited in this specificationincludes all values from at least the lower value without an upperlimit, and all values up to the upper value without a lower limit. Theseare only examples of what is specifically intended, and all possiblecombinations of numerical values between and including the lowest valueand the highest value enumerated are to be considered to be expresslystated in this application.

It also is to be understood that the invention is not limited in itsapplication to the details of construction and the arrangement ofcomponents set forth in the description. Also, it is to be understoodthat the phraseology and terminology used in this specification is forthe purpose of description and should not be regarded as limiting. Theuse of the terms “a” and “an” and “the” and similar referents in thecontext of describing the invention are to be construed to cover boththe singular and the plural, unless otherwise indicated in thisspecification or clearly contradicted by context. The terms“comprising,” “having,” “including,” and “containing” are to beconstrued as open-ended terms (i.e., meaning “including but not limitedto”) unless otherwise noted. All methods described in this specificationcan be performed in any suitable order unless otherwise indicated inthis specification or otherwise clearly contradicted by context. Patentapplications, patents and literature references cited here arespecifically and completely incorporated by reference in their entirety.Where inconsistent interpretations are possible, the present disclosurecontrols.

The use of any and all examples, or exemplary language (e.g., “such as”)provided here, is intended merely to illustrate aspects and embodimentsof the disclosure and does not limit the scope of the claims.

EXAMPLES Example 1 Materials and Methods

Reagents.

Pyrethrins were supplied as a 20% Manufacturing Use Product or “MUP”(PyGanic® MUP 20, MGK (Minneapolis, Minn.). Mineral oil was supplied byBrenntag Great Lakes, LLC. Diluents were supplied by Stepan Company,Procter & Gamble Chemicals, and Vertec Biosolvents. Insecticides werepurchased from Sigma Aldrich (St. Louis, Mo.). Essential oils orbotanicals were purchased from The Good Scents Company, The LebermuthCompany, and Takasago International Corporation. Perilla oil componentsand insecticides were obtained from Sigma Aldrich (St. Louis, Mo.) orCity Chemical (West Haven, Conn.).

Topical Bioassay Method.

Adult mosquitoes were reared on 10% sucrose solution in an insectarymaintained at 27° C., 45% RH and 12/12 hr light/dark photoperiod. Adultfemale Aedes aegypti mosquitoes were segregated in 18″×18″ screen cagesbased on date of eclosion, therefore the exact age of the mosquitoeswere known for bioassays.

Ten female mosquitoes, aged four to six days after eclosion, wereaspirated out of their respective cage and into a small glass jar. Themosquitoes were then anesthetized with CO₂ gas for 30 seconds. After theadults were anesthetized, they were quickly placed on a plastic platformfor treatment application. Treatments were serially diluted (using aBrandTech Scientific Transferpette S pipette (100-1000 μL), labeledcentrifuge tubes, and a vortex mixer) from stocks of insecticides usingreagent grade acetone as the diluent to concentrations as indicated foreach treatment solution. A treatment solution may contain additionalingredients as indicated for each study.

Using a Hamilton PB00-1 Repeating Dispenser with a Hamilton 25Microliter Syringe, 0.5 μL of each treatment solution was applied to thethorax of each mosquito. Immediately following the application of thetreatment, the mosquitoes were gently transferred into a clean paper cupand covered with screen. The mesh screen prevented the mosquitoes fromescaping and allowed the specimens to be viewed for ratings. A cottonball soaked with 10% sucrose solution was inserted into a side hole ofeach cup for hydration and nourishment. Each treatment variable in thestudy was replicated three times using separate cups for eachreplication.

In each study, an untreated control and an acetone treated control wasincluded to ensure that the CO₂ gas and the acetone diluent had nolethal effect on the mosquitoes. The untreated controls treatments wereanesthetized for 30 seconds and gently transferred to the paper cups.The acetone treated control was treated exactly as described aboveexcept that the solution applied to each mosquito was undiluted acetone.

The condition of the mosquitoes in each cup was recorded at one hour and24 hours after initial treatment. The condition classifications usedwere (1) alive and flying, (2) alive and unable to fly, or (3) dead. Thepercent mortality for each treatment was calculated by summing themortalities of each replicate then calculating the percent dead from thetotal number of mosquitoes.

Statistical Analysis.

Where indicated, the mortality data were subjected to probit analysisusing the Statistical Analysis System Version 9.1 program PROC PROBIT(SAS Institute (2003) PROC user's manual, version 9.1. SAS Institute,Cary, N.C.). This analysis estimates an LD₅₀ value or the dose necessaryto achieve 50% mortality. In all cases the likelihood ratio (L.R.) orPearson chi-square goodness-of-fit values indicated that the dataadequately conformed to the probit model (ibid).

Mosquito Stocks for Field Trials.

The Culex and Aedes adult mosquitoes for the field trial were rearedfrom pupae shipped overnight from the Clarke Technical Center Insectaryto the Florida Research Laboratory. Mosquitoes were fed a 10% sugarwater solution upon emergence and were maintained on 10% sugar waterthroughout the field trials. For laboratory experiments and assays, thedesired number of adult mosquitoes (typically about 3-7 days old) wereisolated and maintained on 10% sugar water solution.

Example 2

Perilla leaf oil was tested for efficacy against 3- to 5-day old adultAedes aegypti. Solutions tested included Perilla oil at 1%, 2%, 4%, 6%,8%, and 10%. At 1 hour we obtained 0%, 37%, 97%, 93%, 100%, and 100%knockdown, respectively. At 24 hours we obtained 0%, 20%, 83%, 93%,100%, and 100% mortality, respectively. The CO₂ control and acetonestandard both had 0% knockdown at 1 hour, and 0% mortality at 24 hours.These data suggest that perilla leaf oil exposure by contact leads toAedes aegypti mortality.

Example 3

Perilla leaf oil at concentrations of 1%, 5%, and 10% was tested forefficacy against 1- to 2-day old adult Culex quinquefasciatus. At 1 hourwe obtained 17%, 100%, and 100% knockdown, respectively. At 24 hours weobtained 10%, 100%, and 100% mortality, respectively. The CO₂ controlhad 0% knockdown at 1 hour, and 0% mortality at 24 hours. The acetonestandard had 17% knockdown at 1 hour, and 20% mean mortality at 24hours. These data suggest that perilla leaf oil exposure by contactleads to Culex quinquefasciatus mortality.

Example 4

Perilla seed oil at concentrations of 1%, 5%, 10%, and 20% was testedfor efficacy against 4- to 6-day old adult Aedes aegypti. At 1 hour weobtained 7%, 77%, 83%, and 87% knockdown, respectively. At 24 hours weobtained 0%, 23%, 30%, and 77% mortality, respectively. The CO₂ controland acetone standard both had 0% knockdown at 1 hour, and 0% mortalityat 24 hours. These data suggest that relatively high rates of perillaseed oil exposure by contact, leads to mosquito mortality.

Example 5

Perilla seed oil at concentrations of 1%, 5%, 10%, and 20% was againtested for efficacy against 4- to 6-day old adult Aedes aegypti. At 1hour we obtained 0%, 63%, 87%, and 93% knockdown, respectively. At 24hours we obtained 0%, 20%, 77%, and 90% mortality, respectively. The CO₂control had 0% knockdown at 1 hour, and 0% mortality at 24 hours. Theacetone standard had 7% knockdown at 1 hour, and 7% mean mortality at 24hours. These data suggest that relatively high rates of perilla seed oilexposure by contact, leads to mosquito mortality.

Example 6

Linolenic acid at concentrations of 1%, 5%, 10%, and 20% was tested forefficacy against 4- to 6-day old adult Aedes aegypti. At 1 hour weobtained 0%, 27%, 40%, and 93% knockdown, respectively. At 24 hours weobtained 3%, 33%, 83%, and 93% mortality, respectively. The CO₂ controlhad 0% knockdown at 1 hour, and 7% mortality at 24 hours. The acetonestandard had 0% knockdown at 1 hour, and 0% mortality at 24 hours. Thesedata suggest that relatively high rates of linolenic acid exposure bycontact, leads to mosquito mortality.

Example 7 (S)-(−)-Perillaldehyde at concentrations of 1%, 5%, 10%, and20% was tested for efficacy against 4- to 6-day old adult Aedes aegypti.At 1 hour we obtained 3%, 93%, 100%, and 97% knockdown, respectively. At24 hours we obtained 7%, 93%, 100%, and 100% mortality, respectively.The CO₂ control had 0% knockdown at 1 hour, and 7% mortality at 24hours. The acetone standard had 0% knockdown at 1 hour, and 0% mortalityat 24 hours. These data suggest that perillaldehyde exposure by contactleads to mosquito mortality. Example 8

Farnesene at concentrations of 1%, 5%, 10%, and 20% was tested forefficacy against 4- to 6-day old adult Aedes aegypti. At 1 hour weobtained 0%, 0%, 87%, and 100% knockdown, respectively. At 24 hours weobtained 3%, 13%, 70%, and 100% mortality, respectively. The CO₂ controlhad 0% knockdown at 1 hour, and 7% mortality at 24 hours. The acetonestandard had 0% knockdown at 1 hour, and 0% mortality at 24 hours. Thesedata suggest that relatively high rates of farnesene exposure by contactleads to mosquito mortality.

Example 9

β-Caryophyllene at concentrations of 1%, 5%, 10%, and 20% was tested forefficacy against 4- to 6-day old adult Aedes aegypti. At 1 hour weobtained 0%, 10%, 57%, and 93% knockdown, respectively. At 24 hours weobtained 0%, 17%, 40%, and 83% mortality, respectively. The CO₂ controlhad 0% knockdown at 1 hour, and 7% mortality at 24 hours. The acetonestandard had 0% knockdown at 1 hour, and 0% mortality at 24 hours. Thesedata suggest that β-caryophyllene exposure by contact, leads to mosquitomortality.

Example 10

Dinotefuran and perilla oil were tested for efficacy against 5- to 7-dayold adult Aedes aegypti. Solutions tested included Solution 1 (0.06μg/mosquito of dinotefuran), Solution 2 (3% perilla oil), and Solution 3(0.06 μg/mosquito of dinotefuran with 3% perilla oil). At 1 hour weobtained 37%, 83%, and 97% knockdown for Solutions 1, 2, and 3,respectively. At 24 hours we obtained 57%, 73%, and 97% mortalityrespectively. The CO₂ control and acetone standard both had 0% knockdownat 1 hour, and 0% mortality at 24 hours. Results are shown in Table 2.

TABLE 2 Efficacy of perilla oil, dinotefuran, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS PERILLA OIL 3% 57DINOTEFURAN 0.06 μg 73 OBS.* CALC.** PERILLA OIL + 3% + 0.06 μg 97^(‡)88.39 DINOTEFURAN *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ^(‡)Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

Example 11

Dinotefuran and perilla oil were tested for efficacy against 4- to 6-dayold adult Aedes aegypti. Solutions tested included Solution 1 (2%perilla oil), Solution 2 (0.004 μg/mosquito dinotefuran with 2% perillaoil), Solution 3 (0.006 μg/mosquito dinotefuran with 2% perilla oil),and Solution 4 (0.008 μg/mosquito of dinotefuran with 2% perilla oil).At 1 hour we obtained 13%, 87%, 80%, and 90% knockdown for Solutions 1,2, 3, and 4, respectively. At 24 hours we obtained 0%, 77%, 77%, and 90%mortality respectively. The CO₂ control and acetone standard both had 0%knockdown at 1 hour and 0% mortality at 24 hours. Dinotefuran was testedat discriminating doses 7.5 to 15 times lower that the LD₅₀ of 0.06μg/mosquito. These data suggest that the application of dinotefuran andperilla oil together leads to an increase in mortality over theapplication of perilla oil alone.

Example 12

Dinotefuran and perilla oil were tested individually and in combinationfor efficacy against 3- to 5-day old adult Aedes aegypti wheredinotefuran was tested at discriminating doses 7.5 to 15 times lowerthan the LD₅₀ of 0.06 μg/mosquito. Results are shown in Table 3 andTable 4.

TABLE 3 Efficacy data for dinotefuran and perilla oil testedindividually and in combination. 1 hour 24 hour Treatment knockdownmortality CO₂ Control 0% 0% Acetone Standard 0% 0% 3% Perilla oil 40%60% 0.004 μg/mosquito dinotefuran 0% 0% 0.006 μg/mosquito dinotefuran 0%0% 0.008 μg/mosquito dinotefuran 17% 0% 0.004 μg/mosquito dinotefuran +3% Perilla Oil 100% 90% 0.006 μg/mosquito dinotefuran + 3% Perilla Oil100% 97% 0.008 μg/mosquito dinotefuran + 3% Perilla Oil 100% 93%

TABLE 4 Efficacy of perilla oil, dinotefuran, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS PERILLA OIL 3%^(T) 60DINOTEFURAN 0.004 μg 0 OBS.* CALC.** PERILLA OIL + 3% + 0.004 μg 90^(‡)60 DINOTEFURAN PERILLA OIL 3% 60 DINOTEFURAN 0.006 μg 0 OBS.* CALC.**PERILLA OIL + 3% + 0.006 μg 97^(‡) 60 DINOTEFURAN PERILLA OIL 3% 60DINOTEFURAN 0.008 μg 0 OBS.* CALC.** PERILLA OIL + 3% + 0.008 μg 93^(‡)60 DINOTEFURAN ^(T)3% efficacy was derived from data that underwentprobit analysis to predict lethal dose values from topical applicationbioassay. *Obs. = observed efficacy **Calc. = efficacy calculated usingColby (1967) formula ^(‡)Since the actual insecticidal kill rate exceedsthe calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

Example 13

Solution 1 (2% of perillaldehyde), Solution 2 (0.008 μg/mosquito ofdinotefuran), and Solution 3 (0.008 μg/mosquito of dinotefuran with 2%of perillaldehyde) were tested for efficacy against 3- to 5-day oldadult Culex quinquefasciatus. At 1 hour we obtained 33%, 10%, and 100%knockdown for Solutions 1, 2, and 3, respectively. At 24 hours weobtained 13%, 77%, and 100% mortality for Solutions 1, 2, and 3,respectively. The CO₂ control and acetone standard both had 0% knockdownat 1 hour, and 0% mortality at 24 hours. Results are shown in Table 5.

TABLE 5 Efficacy of perillaldehyde, dinotefuran, and a combination ofboth against adult, virgin, female Culex quinquefasciatus mosquitoes. %MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS PERILLALDEHYDE 2%13 DINOTEFURAN 0.008 μg 77 OBS.* CALC.** PERILLALDEHYDE + 2% + 0.008 μg100^(‡) 79.99 DINOTEFURAN *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ^(‡)Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

Example 14

In support of example 2, Solution 1 (0.008 μg/mosquito of dinotefuran)and Solution 2 (0.008 μg/mosquito of dinotefuran with 2% ofperillaldehyde) were tested for efficacy against 3- to 5-day old adultCulex quinquefasciatus. At 1 hour we obtained 10% and 90% knockdown forSolution 1 and 2, respectively. At 24 hours we obtained 73% and 90%mortality for Solution 1 and 2, respectively. The CO₂ control andacetone standard both had 0% knockdown at 1 hour, and 0% mortality at 24hours.

Example 15

In support of examples 2 and 3, Solution 1 (0.008 μg/mosquito ofdinotefuran with 3% of perillaldehyde) was tested for efficacy against4- to 6-day old adult Culex quinquefasciatus. At 1 hour we obtained 100%knockdown; and at 24 hours we obtained 100% mortality. The CO₂ controland acetone standard both had 0% knockdown at 1 hour, and 0% mortalityat 24 hours.

Example 16

Dinotefuran and perillaldehyde were tested individually and incombination for efficacy against 3- to 5-day old adult Aedes aegyptiwhere dinotefuran was tested at discriminating doses 7.5 to 15 timeslower than the LD₅₀ of 0.06 μg/mosquito. Results are shown in Table 6and Table 7.

TABLE 6 Efficacy data for dinotefuran and perillaldehyde testedindividually and in combination. 1 hour 24 hour Treatment knockdownmortality CO₂ Control 0% 0% Acetone Standard 0% 0% 3% Perillaldehyde 53%43% 0.004 μg/mosquito dinotefuran 0% 0% 0.006 μg/mosquito dinotefuran 3%3% 0.008 μg/mosquito dinotefuran 3% 13% 0.06 μg/mosquito dinotefuran 77%53% 0.004 μg/mosquito dinotefuran + 3% 100% 93% Perillaldehyde 0.006μg/mosquito dinotefuran + 3% 100% 97% Perillaldehyde 0.008 μg/mosquitodinotefuran + 3% 93% 93% Perillaldehyde 0.06 μg/mosquito dinotefuran +3% 100% 100% Perillaldehyde

TABLE 7 Efficacy of perillaldehyde, dinotefuran, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN-PERCENT EFFICACY ACTIVE INGREDIENT TRATION AFTER 24 HRS PERILLALDEHYDE3% 43 DINOTEFURAN 0.06 μg 53 OBS.* CALC.** PERILLALDEHYDE + 3% + 0.06 μg100 ‡  73.21 DINOTEFURAN PERILLALDEHYDE 3% 43 DINOTEFURAN 0.004 μg 0OBS.* CALC.** PERILLALDEHYDE + 3% + 0.004 μg 93 ‡ 43 DINOTEFURANPERILLALDEHYDE 3% 43 DINOTEFURAN 0.006 μg 3 OBS.* CALC.**PERILLALDEHYDE + 3% + 0.006 μg 97 ‡ 44.71 DINOTEFURAN PERILLALDEHYDE 3%43 DINOTEFURAN 0.008 μg 13 OBS.* CALC.** PERILLALDEHYDE + 3% + 0.008 μg93 ‡ 50.41 DINOTEFURAN *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡ Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

Example 17

Dinotefuran and linolenic acid were tested for efficacy against 4- to6-day old adult Aedes aegypti. For the following concentrations 3%linolenic acid, 0.06 μg/mosquito of dinotefuran, and 0.06 μg/mosquito ofdinotefuran with 3% linolenic acid, at 1 hour we obtained 17%, 50%, and100% knockdown respectively. At 24 hours we obtained 3%, 47%, and 100%mortality respectively. The CO₂ control and acetone standard both had 0%knockdown at 1 hour, and 0% mortality at 24 hours. Results are shown inTable 8.

TABLE 8 Efficacy of linolenic acid, dinotefuran, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS LINOLENIC ACID 3% 3DINOTEFURAN 0.06 μg 47 OBS.* CALC.** LINOLENIC ACID + 3% + 0.06 μg 100‡48.59 DINOTEFURAN *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

Example 18

Dinotefuran and β-caryophyllene were tested for efficacy against 4- to6-day old adult Aedes aegypti. For the following concentrations 3%β-caryophyllene, 0.06 μg/mosquito of dinotefuran, and 0.06 μg/mosquitoof dinotefuran with 3% β-caryophyllene, at 1 hour we obtained 3%, 50%,and 100% knockdown respectively. At 24 hours we obtained 3%, 47%, and100% mortality respectively. The CO₂ control and acetone standard bothhad 0% knockdown at 1 hour, and 0% mortality at 24 hours. Results areshown in Table 9.

TABLE 9 Efficacy of β-caryophyllene, dinotefuran, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS β-CARYOPHYLLENE 3% 3DINOTEFURAN 0.06 μg 47 OBS.* CALC.** β-CARYOPHYLLENE + 3% + 0.06 μg 100‡48.59 DINOTEFURAN *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

Example 19

Dinotefuran and farnesene were tested for efficacy against 4- to 6-dayold adult Aedes aegypti. For the following concentrations 3% farnesene,0.06 μg/mosquito of dinotefuran, and 0.06 μg/mosquito of dinotefuranwith 3% farnesene, at 1 hour we obtained 3%, 50%, and 97% knockdownrespectively. At 24 hours we obtained 7%, 47%, and 97% mean mortalityrespectively. The CO₂ control and acetone standard both had 0% knockdownat 1 hour, and 0% mean mortality at 24 hours. Results are shown in Table10.

TABLE 10 Efficacy of farnesene, dinotefuran, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS FARNESENE 3% 7DINOTEFURAN 0.06 μg 47 OBS.* CALC.** FARNESENE + DINOTEFURAN 3% + 0.06μg 97‡ 50.71 *Obs. = observed efficacy **Calc. = efficacy calculatedusing Colby (1967) formula ‡Since the actual insecticidal kill rateexceeds the calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

Example 20

Permethrin and perillaldehyde were tested for efficacy against 4- to6-day old adult Aedes aegypti. For the following concentrations 3%perillaldehyde, 0.0004 μg/mosquito of permethrin, and 0.0004 μg/mosquitoof permethrin with 3% perillaldehyde, at 1 hour we obtained 10%, 93%,and 100% knockdown respectively. At 24 hours we obtained 10%, 70%, and100% mortality respectively. The CO₂ control had 0% knockdown at 1 hour,and 0% mortality at 24 hours. The acetone standard had 3% knockdown at 1hour, and 7% mortality at 24 hours. Results are shown in Table 11.

TABLE 11 Efficacy of perillaldehyde, permethrin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS PERILLALDEHYDE 3% 10PERMETHRIN 0.0004 μg 70 OBS.* CALC.** PERILLALDEHYDE + 3% + 0.0004 μg100‡ 79.30 PERMETHRIN *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

Example 21

Permethrin and farnesene were tested for efficacy against 4- to 6-dayold adult Aedes aegypti. For the following concentrations 3% farnesene,0.0004 μg/mosquito of permethrin, and 0.0004 μg/mosquito of permethrinwith 3% farnesene, at 1 hour we obtained 0%, 93%, and 20% knockdownrespectively. At 24 hours we obtained 0%, 70%, and 47% mortalityrespectively. The CO₂ control had 0% knockdown at 1 hour, and 0%mortality at 24 hours. The acetone standard had 3% knockdown at 1 hour,and 7% mortality at 24 hours. Results are shown in Table 12.

TABLE 12 Efficacy of farnesene, permethrin, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS FARNESENE 3% 0PERMETHRIN 0.0004 μg 70 OBS.* CALC.** FARNESENE + PERMETHRIN 3% + 0.0004μg 47‡ 70 *Obs. = observed efficacy **Calc. = efficacy calculated usingColby (1967) formula ‡Since the calculated insecticidal kill rateexceeds the observed value, then the action of the combination isantagonistic.

Example 22

Permethrin and linolenic acid were tested for efficacy against 4- to6-day old adult Aedes aegypti. For the following concentrations 3%linolenic acid, 0.0004 μg/mosquito of permethrin, and 0.0004 μg/mosquitoof permethrin with 3% linolenic acid, at 1 hour we obtained 7%, 93%, and77% knockdown respectively. At 24 hours we obtained 60%, 70%, and 63%mortality respectively. The CO₂ control had 0% knockdown at 1 hour, and0% mortality at 24 hours. The acetone standard had 3% knockdown at 1hour, and 7% mortality at 24 hours. Results are shown in Table 13.

TABLE 13 Efficacy of linolenic acid, permethrin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS LINOLENIC ACID 3% 60PERMETHRIN 0.0004 μg 70 OBS.* CALC.** LINOLENIC ACID + 3% + 0.0004 μg63‡ 88 PERMETHRIN *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the calculated insecticidalkill rate exceeds the observed value, then the action of the combinationis antagonistic.

Example 23

Permethrin and β-caryophyllene were tested for efficacy against 4- to6-day old adult Aedes aegypti. For the following concentrations 3%β-caryophyllene, 0.0004 μg/mosquito of permethrin, and 0.0004μg/mosquito of permethrin with 3% β-caryophyllene, at 1 hour we obtained0%, 93%, and 43% knockdown respectively. At 24 hours we obtained 10%,70%, and 43% mean mortality respectively. The CO₂ control had 0%knockdown at 1 hour, and 0% mean mortality at 24 hours. The acetonestandard had 3% knockdown at 1 hour, and 7% mean mortality at 24 hours.Results are shown in Table 14.

TABLE 14 Efficacy of β-caryophyllene, permethrin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS β-CARYOPHYLLENE 3% 10PERMETHRIN 0.0004 μg 70 OBS.* CALC.** β-CARYOPHYLLENE + 3% + 0.0004 μg43‡ 79.40 PERMETHRIN *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the calculated insecticidalkill rate exceeds the observed value, then the action of the combinationis antagonistic.

Example 24

Pyrethrin and perilla oil were tested for efficacy against 3- to 5-dayold adult Aedes aegypti. Solutions tested included Solution 1 (0.0001μg/mosquito of pyrethrin with 1% perilla oil), Solution 2 (0.0001μg/mosquito of pyrethrin with 5% perilla oil), Solution 3 (0.0001μg/mosquito of pyrethrin with 10% perilla oil), Solution 4 (0.001μg/mosquito of pyrethrin with 1% perilla oil), Solution 5 (0.001μg/mosquito of pyrethrin with 5% perilla oil), and Solution 6 (0.001μg/mosquito of pyrethrin with 10% perilla oil). At 1 hour we obtained0%, 100%, 100%, 70%, 93% and 97% knockdown for Solutions 1, 2, 3, 4, 5,and 6, respectively. At 24 hours we obtained 3%, 93%, 97%, 57%, 87%,93%, and 93% mortality, respectively. The CO₂ control and acetonestandard both had 0% knockdown at 1 hour, and 0% mortality at 24 hours.These data suggest that increased rates of both pyrethrin and perillaoil, applied together, results in greater mortality.

Example 25

Pyrethrin and β-caryophyllene were tested for efficacy against 4- to6-day old adult Aedes aegypti. For the following concentrations 3%β-caryophyllene, 0.002 μg/mosquito of pyrethrin, and 0.002 μg/mosquitoof pyrethrin with 3% β-caryophyllene, at 1 hour we obtained 0%, 90%, and100% knockdown respectively. At 24 hours we obtained 20%, 57%, and 97%mortality respectively. The CO₂ control and acetone standard both had 0%knockdown at 1 hour, and 0% mortality at 24 hours. Results are shown inTable 15.

TABLE 15 Efficacy of β-caryophyllene, pyrethrin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS β-CARYOPHYLLENE 3% 20PYRETHRIN 0.002 μg 57 OBS.* CALC.** β-CARYOPHYLLENE + 3% + 0.002 μg 97‡65.60 PYRETHRIN *Obs. = observed efficacy **Calc. = efficacy calculatedusing Colby (1967) formula ‡Since the actual insecticidal kill rateexceeds the calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

Example 26

Pyrethrin and farnesene were tested for efficacy against 4- to 6-day oldadult Aedes aegypti. For the following concentrations 3% farnesene,0.002 μg/mosquito of pyrethrin, and 0.002 μg/mosquito of pyrethrin with3% farnesene, at 1 hour we obtained 0%, 90%, and 83% knockdownrespectively. At 24 hours we obtained 0%, 57%, and 73% mortalityrespectively. The CO₂ control and acetone standard both had 0% knockdownat 1 hour, and 0% mortality at 24 hours. Results are shown in Table 16.

TABLE 16 Efficacy of farnesene, pyrethrin, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS FARNESENE 3% 0PYRETHRIN 0.002 μg 57 OBS.* CALC.** FARNESENE + PYRETHRIN 3% + 0.002 μg73‡ 57 *Obs. = observed efficacy **Calc. = efficacy calculated usingColby (1967) formula ‡Since the actual insecticidal kill rate exceedsthe calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

Example 27

We tested pyrethrin+linolenic acid for efficacy against 4- to 6-day oldadult Aedes aegypti. For the following concentrations 3% linolenic acid,0.002 μg/mosquito of pyrethrin, and 0.002 μg/mosquito of pyrethrin with3% linolenic acid, at 1 hour we obtained 17%, 90%, and 50% knockdownrespectively. At 24 hours we obtained 7%, 57%, and 37% mean mortalityrespectively. The CO₂ control and acetone standard both had 0% knockdownat 1 hour, and 0% mean mortality at 24 hours. Results are shown in Table17.

TABLE 17 Efficacy of linolenic acid, pyrethrin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS LINOLENIC ACID 3% 7PYRETHRIN 0.002 μg 57 OBS.* CALC.** LINOLENIC ACID + 3% + 0.002 μg 37‡60.01 PYRETHRIN *Obs. = observed efficacy **Calc. = efficacy calculatedusing Colby (1967) formula ‡Since the calculated insecticidal kill rateexceeds the observed value, then the action of the combination isantagonistic.

Example 28

We tested pyrethrin+perillaldehyde for efficacy against 3- to 5-day oldadult Culex quinquefasciatus. For the concentration, 2% ofperillaldehyde, and 0.001 μg/mosquito of pyrethrin, and 0.001μg/mosquito of pyrethrin with 2% of perillaldehyde, at 1 hour weobtained 33%, 10%, and 80% knockdown respectively. At 24 hours weobtained 13%, 7%, and 33% mean mortality respectively. The CO₂ controland acetone standard both had 0% knockdown at 1 hour, and 0% meanmortality at 24 hours. Results are shown in Table 18.

TABLE 18 Efficacy of perillaldehyde, pyrethrin, and a combination ofboth against adult, virgin, female Culex quinquefasciatus mosquitoes.CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRSPERILLALDEHYDE 3% 13 PYRETHRIN 0.001 μg 7 OBS.* CALC.** PERILLALDEHYDE +3% + 0.001 μg 33‡ 19.09 PYRETHRIN *Obs. = observed efficacy **Calc. =efficacy calculated using Colby (1967) formula ‡Since the actualinsecticidal kill rate exceeds the calculated value, then the action ofthe combination is super-additive or a synergistic effect is present.

Example 29

Etofenprox and perilla oil were tested for efficacy against 5- to 7-dayold adult Aedes aegypti. Solutions tested included Solution 1 (0.001μg/mosquito of etofenprox), Solution 2 (3% perilla oil), and Solution 3(0.001 μg/mosquito of etofenprox with 3% perilla oil). At 1 hour weobtained 73%, 83%, and 87% knockdown respectively. At 24 hours weobtained 40%, 73%, and 87% mortality respectively. The CO₂ control andacetone standard both had 0% knockdown at 1 hour, and 0% mortality at 24hours. Results are shown in Table 19.

TABLE 19 Efficacy of perilla oil, etofenprox, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS PERILLA OIL 3% 73ETOFENPROX 0.001 μg 40 OBS.* CALC.** PERILLA OIL + ETOFENPROX 3% + 0.001μg 87‡ 83.8 *Obs. = observed efficacy **Calc. = efficacy calculatedusing Colby (1967) formula ‡Since the actual insecticidal kill rateexceeds the calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

Example 30

Etofenprox and perillaldehyde were tested for efficacy against 3- to5-day old adult Aedes aegypti. For the following concentrations 3%perillaldehyde, 0.002 μg/mosquito of etofenprox, and 0.002 μg/mosquitoof etofenprox with 3% perillaldehyde, at 1 hour we obtained 90%, 83%,and 93% knockdown respectively. At 24 hours we obtained 77%, 53%, and93% mortality respectively. The CO₂ control and acetone standard bothhad 0% knockdown at 1 hour, and 0% mortality at 24 hours. Results areshown in Table 20.

TABLE 20 Efficacy of perillaldehyde, etofenprox, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS PERILLALDEHYDE 3% 77ETOFENPROX 0.002 μg 53 OBS.* CALC.** PERILLALDEHYDE + 3% + 0.002 μg 93‡89.19 ETOFENPROX *Obs. = observed efficacy **Calc. = efficacy calculatedusing Colby (1967) formula ‡Since the actual insecticidal kill rateexceeds the calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

Example 31

Etofenprox and farnesene were tested for efficacy against 3- to 5-dayold adult Aedes aegypti. For the following concentrations 3% farnesene,0.002 μg/mosquito of etofenprox, and 0.002 μg/mosquito of etofenproxwith 3% farnesene, at 1 hour we obtained 7%, 83%, and 60% knockdownrespectively. At 24 hours we obtained 13%, 53%, and 50% mortalityrespectively. The CO₂ control and acetone standard both had 0% knockdownat 1 hour, and 0% mortality at 24 hours. Results are shown in Table 21.

TABLE 21 Efficacy of farnesene, etofenprox, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS FARNESENE 3% 13ETOFENPROX 0.002 μg 53 OBS.* CALC.** FARNESENE + ETOFENPROX 3% + 0.002μg 50‡ 59.11 *Obs. = observed efficacy **Calc. = efficacy calculatedusing Colby (1967) formula ‡Since the calculated insecticidal kill rateexceeds the observed value, then the action of the combination isantagonistic.

Example 32

Etofenprox and β-caryophyllene were tested for efficacy against 3- to5-day old adult Aedes aegypti. For the following concentrations 3%β-caryophyllene, 0.002 μg/mosquito of etofenprox, and 0.002 μg/mosquitoof etofenprox with 3% β-caryophyllene, at 1 hour we obtained 13%, 83%,and 87% knockdown respectively. At 24 hours we obtained 3%, 53%, and 77%mortality respectively. The CO₂ control and acetone standard both had 0%knockdown at 1 hour, and 0% mortality at 24 hours. Results are shown inTable 22.

TABLE 22 Efficacy of β-caryophyllene, etofenprox, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS β-CARYOPHYLLENE 3% 77ETOFENPROX 0.002 μg 53 OBS.* CALC.** β-CARYOPHYLLENE + 3% + 0.002 μg93^(‡) 89.19 ETOFENPROX *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ^(‡)Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

Example 33

We tested etofenprox+linolenic acid for efficacy against 3- to 5-day oldadult Aedes aegypti. For the following concentrations 3% linolenic acid,0.002 μg/mosquito of etofenprox, and 0.002 μg/mosquito of etofenproxwith 3% linolenic acid, at 1 hour we obtained 0%, 83%, and 0% knockdownrespectively. At 24 hours we obtained 3%, 53%, and 7% mean mortalityrespectively. The CO₂ control and acetone standard both had 0% knockdownat 1 hour, and 0% mean mortality at 24 hours. Results are shown in Table23.

TABLE 23 Efficacy of linolenic acid, etofenprox, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS LINOLENIC ACID 3% 3ETOFENPROX 0.002 μg 53 OBS.* CALC.** LINOLENIC ACID + 3% + 0.002 μg7^(‡) 54.41 ETOFENPROX *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ^(‡)Since the calculatedinsecticidal kill rate exceeds the observed value, then the action ofthe combination is antagonistic.

Example 34

Ethiprole and perilla oil were tested individually and in combinationfor efficacy against 4- to 6-day old adult Aedes aegypti. Solutionstested included Solution 1 (0.0005 μg/mosquito of ethiprole), Solution 2(2% perilla oil), and Solution 3 (0.0005 μg/mosquito of ethiprole with2% perilla oil). At 1 hour we obtained 0%, 13%, and 40% knockdown,respectively. At 24 hours we obtained 97%, 0%, and 47% mean mortality,respectively. The CO₂ control and acetone standard both had 0% knockdownat 1 hour, and 0% mean mortality at 24 hours. Results are shown in Table24.

TABLE 24 Efficacy of perilla oil, etofenprox, a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS PERILLA OIL 2% 0 ETOFENPROX0.0005 μg 97 OBS.* CALC.** PERILLA OIL + 2% + 0.0005 μg 47^(‡) 97ETOFENPROX *Obs. = observed efficacy **Calc. = efficacy calculated usingColby (1967) formula ^(‡)Since the calculated insecticidal kill rateexceeds the observed value, then the action of the combination isantagonistic.

Example 35

Various perilla oil components, perillaldehyde analogs, and insecticideswere tested for efficacy against mosquitoes as detailed in ReferenceExample 1 with results shown in Tables 25-35.

TABLE 25 Efficacy of perilla oil, clothianidin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Perilla Oil 1% 3Clothianidin 0.005 μg 7 OBS.* CALC.** Perilla Oil + Clothianidin 1% +0.005 μg 77_(‡) 9.79 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡)Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 26 Efficacy of perillaldehyde, clothianidin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Perillaldehyde 2% 30Clothianidin 0.025 μg 40 OBS.* CALC.** Perillaldehyde + 2% + 0.025 μg97_(‡) 58 Clothianidin *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡)Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 27 Efficacy of β-caryophyllene, clothianidin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS β-caryophyllene 3% 10Clothianidin 0.01 μg 50 OBS.* CALC.** β-caryophyllene + 3% + 0.01 μg90_(‡) 55 Clothianidin *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡)Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 28 Efficacy of farnesene, clothianidin, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Farnesene 3% 3 Clothianidin0.01 μg 43 OBS.* CALC.** Farnesene + 3% + 0.01 μg 93_(‡) 44.71Clothianidin *Obs. = observed efficacy **Calc. = efficacy calculatedusing Colby (1967) formula _(‡)Since the actual insecticidal kill rateexceeds the calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

TABLE 29 Efficacy of linolenic acid, clothianidin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Linolenic Acid 3% 13Clothianidin 0.01 μg 43 OBS.* CALC.** Linolenic Acid + 3% + 0.01 μg80_(‡) 49.11 Clothianidin *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡)Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 30 Efficacy of limonene, clothianidin, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Limonene 5% 27 Clothianidin0.025 μg 20 OBS.* CALC.** Limonene + Clothianidin 5% + 0.025 μg _(‡)10041.6 *Obs. = observed efficacy **Calc. = efficacy calculated using Colby(1967) formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 31 Efficacy of (R)-(−)-carvone, clothianidin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS (R)-(−)-carvone 3% 7Clothianidin 0.025 μg 20 OBS.* CALC.** (R)-(−)-carvone + 3% + 0.025 μg_(‡)100 25.6 Clothianidin *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡)Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 32 Efficacy of (S)-(+)-carvone, clothianidin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS (S)-(+)-carvone 3% 13Clothianidin 0.025 μg 20 OBS.* CALC.** (S)-(+)-carvone + 3% + 0.025 μg_(‡)97 30.4 Clothianidin *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡)Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 33 Efficacy of (1R)-(−)-myrtenal, clothianidin, and a combinationof both against adult, virgin, female Aedes aegypti mosquitoes. %MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS (1R)-(−)-myrtenal2% 10 Clothianidin 0.025 μg 20 OBS.* CALC.** (1R)-(−)-myrtenal + 2% +0.025 μg _(‡)93 28 Clothianidin *Obs. = observed efficacy **Calc. =efficacy calculated using Colby (1967) formula _(‡)Since the actualinsecticidal kill rate exceeds the calculated value, then the action ofthe combination is super-additive or a synergistic effect is present.

TABLE 34 Efficacy of (S)-(−)-perillyl alcohol, clothianidin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS(S)-(−)-perillyl alcohol 2% 70 Clothianidin 0.025 μg 20 OBS.* CALC.**(S)-(−)-perillyl alcohol + 2% + 0.025 μg _(‡)100 76 Clothianidin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 35 Efficacy of (S)-(−)-Perillic acid, clothianidin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS(S)-(−)-Perillic acid 1% 7 Clothianidin 0.025 μg 20 OBS.* CALC.**(S)-(−)-Perillic acid + 1% + 0.025 μg _(‡)57 25.6 Clothianidin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

Example 36

Various perilla oil components, perillaldehyde analogs, and insecticideswere tested for efficacy against mosquitoes as detailed in ReferenceExample 1 with results shown in Tables 36-46.

TABLE 36 Efficacy of D-limonene, Dinotefuran, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS D-limonene 5% 13Dinotefuran 0.06 μg 60 OBS.* CALC.** D-limonene + 5% + 0.06 μg 97_(‡)65.2 Dinotefuran *Obs. = observed efficacy **Calc. = efficacy calculatedusing Colby (1967) formula _(‡)Since the actual insecticidal kill rateexceeds the calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

TABLE 37 Efficacy of (S)-(+)-Carvone, Dinotefuran, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS (S)-(+)-Carvone 3% 33Dinotefuran 0.06 μg 60 OBS.* CALC.** (S)-(+)-Carvone + Dinotefuran 3% +0.06 μg 100‡ 73.2 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 38 Efficacy of (S)-(+)-Carvone, Dinotefuran, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS (S)-(+)-Carvone 3% 37Dinotefuran 0.01 μg 3 OBS.* CALC.** (S)-(+)-Carvone + Dinotefuran 3% +0.01 μg 100‡ 38.89 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 39 Efficacy of (R)-(−)-Carvone, Dinotefuran, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS (R)-(−)-Carvone 3% 33Dinotefuran 0.01 μg 3 OBS.* CALC.** (R)-(−)-Carvone + Dinotefuran 3% +0.01 μg 93‡ 35.01 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 40 Efficacy of (1R)-(−)-Myrtenal, Dinotefuran, and a combinationof both against adult, virgin, female Aedes aegypti mosquitoes. CONCEN-% MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS (1R)-(−)-Myrtenal 2%57 Dinotefuran 0.06 μg 60 OBS.* CALC.** (1R)-(−)-Myrtenal + Dinotefuran2% + 0.06 μg 97‡ 82.8 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 41 Efficacy of (1R)-(−)-Myrtenal, Dinotefuran, and a combinationof both against adult, virgin, female Aedes aegypti mosquitoes. CONCEN-% MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS (1R)-(−)-Myrtenal 2%23 Dinotefuran 0.01 μg 3 OBS.* CALC.** (1R)-(−)-Myrtenal + Dinotefuran2% + 0.01 μg 70‡ 25.31 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 42 Efficacy of (S)-(−)-Perillyl alcohol, Dinotefuran, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS(S)-(−)-Perillyl alcohol 2% 83 Dinotefuran 0.06 μg 60 OBS.* CALC.**(S)-(−)-Perillyl alcohol + 2% + 0.06 μg 100‡ 93.2 Dinotefuran *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 43 Efficacy of (S)-(−)-Perillyl alcohol, Dinotefuran, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS(S)-(−)-Perillyl alcohol 1% 0 Dinotefuran 0.01 μg 0 OBS.* CALC.**(S)-(−)-Perillyl alcohol + 1% + 0.01 μg 83‡ 0 Dinotefuran *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 44 Efficacy of (S)-(−)-Perillic acid, Dinotefuran, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS(S)-(−)-Perillic acid 1% 10 Dinotefuran 0.06 μg 60 OBS.* CALC.**(S)-(−)-Perillic acid + 1% + 0.06 μg 93‡ 64 Dinotefuran *Obs. = observedefficacy **Calc. = efficacy calculated using Colby (1967) formula ‡Sincethe actual insecticidal kill rate exceeds the calculated value, then theaction of the combination is super-additive or a synergistic effect ispresent.

TABLE 45 Efficacy of 3-methyl-1-cyclohexene-1-carboxaldehyde (3-methyl), Dinotefuran, and a combination of both against adult, virgin,female Aedes aegypti mosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENTTRATION AFTER 24 HRS 3-methyl 2% 17 Dinotefuran 0.06 μg 60 OBS.* CALC.**3-methyl + Dinotefuran 2% + 0.06 μg 100‡ 66.8 *Obs. = observed efficacy**Calc. = efficacy calculated using Colby (1967) formula ‡Since theactual insecticidal kill rate exceeds the calculated value, then theaction of the combination is super-additive or a synergistic effect ispresent.

TABLE 46 Efficacy of 3-methyl-1-cyclohexene-1-carboxaldehyde (3-methyl), Dinotefuran, and a combination of both against adult, virgin,female Aedes aegypti mosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENTTRATION AFTER 24 HRS 3-methyl 2% 0 Dinotefuran 0.01 μg 0 OBS.* CALC.**3-methyl + Dinotefuran 2% + 0.01 μg 100‡ 0 *Obs. = observed efficacy**Calc. = efficacy calculated using Colby (1967) formula ‡Since theactual insecticidal kill rate exceeds the calculated value, then theaction of the combination is super-additive or a synergistic effect ispresent.

Example 37

Various perilla oil components, perillaldehyde analogs, and insecticideswere tested for efficacy against mosquitoes as detailed in ReferenceExample 1 with results shown in Tables 47-58.

TABLE 47 Efficacy of Perilla oil, Thiamethoxam, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS Perilla oil 2% 23Thiamethoxam 0.0075 μg 27 OBS.* CALC.** Perilla oil + Thiamethoxam 2% +0.0075 μg 100‡ 43.79 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 48 Efficacy of Perilla oil, Thiamethoxam, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS Perilla oil 2% 23Thiamethoxam 0.0025 μg 3 OBS.* CALC.** Perilla oil + Thiamethoxam 2% +0.0025 μg 90‡ 25.31 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 49 Efficacy of Farnasene, Thiamethoxam, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS Farnasene 3% 3Thiamethoxam 0.0075 μg 37 OBS.* CALC.** Farnasene + Thiamethoxam 3% +0.0075 μg 100‡ 38.89 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 50 Efficacy of (S)-(−)-Perillaldehyde ((S)-Perillaldehyde),Thiamethoxam, and a combination of both against adult, virgin, femaleAedes aegypti mosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATIONAFTER 24 HRS (S)-Perillaldehyde 2% 30 Thiamethoxam 0.0075 μg 43 OBS.*CALC.** (S)-Perillaldehyde + 2% + 0.0075 μg 97‡ 60.1 Thiamethoxam *Obs.= observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 51 Efficacy of Linolenic acid, Thiamethoxam, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS Linolenic acid 3% 13Thiamethoxam 0.0075 μg 37 OBS.* CALC.** Linolenic acid + Thiamethoxam3% + 0.0075 μg 100‡ 45.19 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 52 Efficacy of β-Caryophyllene, Thiamethoxam, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS β-Caryophyllene 3% 10Thiamethoxam 0.0075 μg 30 OBS.* CALC.** β-Caryophyllene + 3% + 0.0075 μg90‡ 37 Thiamethoxam *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 53 Efficacy of D-limonene, Thiamethoxam, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS D-limonene 5% 0Thiamethoxam 0.0075 μg 23 OBS.* CALC.** D-limonene + Thiamethoxam 5% +0.0075 μg 87‡ 23 *Obs. = observed efficacy **Calc. = efficacy calculatedusing Colby (1967) formula ‡Since the actual insecticidal kill rateexceeds the calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

TABLE 54 Efficacy of (R)-(−)-Carvone, Thiamethoxam, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS (R)-(−)-Carvone 3% 0Thiamethoxam 0.0075 μg 23 OBS.* CALC.** (R)-(−)-Carvone + 3% + 0.0075 μg57‡ 23 Thiamethoxam *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 55 Efficacy of (S)-(+)-Carvone, Thiamethoxam, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS (S)-(+)-Carvone 3% 3Thiamethoxam 0.0075 μg 23 OBS.* CALC.** (S)-(+)-Carvone + 3% + 0.0075 μg97‡ 25.31 Thiamethoxam *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 56 Efficacy of (1R)-(−)-Myrtenal, Thiamethoxam, and a combinationof both against adult, virgin, female Aedes aegypti mosquitoes. CONCEN-% MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS (1R)-(−)-Myrtenal 2%0 Thiamethoxam 0.0075 μg 23 OBS.* CALC.** (1R)-(−)-Myrtenal + 2% +0.0075 μg 77‡ 23 Thiamethoxam *Obs. = observed efficacy **Calc. =efficacy calculated using Colby (1967) formula ‡Since the actualinsecticidal kill rate exceeds the calculated value, then the action ofthe combination is super-additive or a synergistic effect is present.

TABLE 57 Efficacy of (S)-(−)-Perillyl alcohol ((S)-Perillyl alcohol),Thiamethoxam, and a combination of both against adult, virgin, femaleAedes aegypti mosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATIONAFTER 24 HRS (S)-Perillyl alcohol 2% 33 Thiamethoxam 0.0075 μg 3 OBS.*CALC.** (S)-Perillyl alcohol + 2% + 0.0075 μg 77‡ 35.01 Thiamethoxam*Obs. = observed efficacy **Calc. = efficacy calculated using Colby(1967) formula ‡Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 58 Efficacy of (S)-(−)-Perillic acid, Thiamethoxam, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS(S)-(−)-Perillic acid 1% 13 Thiamethoxam 0.0075 μg 3 OBS.* CALC.**(S)-(−)-Perillic acid + 1% + 0.0075 μg 20‡ 15.61 Thiamethoxam *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

Example 38

Various perilla oil components, perillaldehyde analogs, and insecticideswere tested for efficacy against mosquitoes as detailed in ReferenceExample 1 with results shown in Tables 59-68.

TABLE 59 Efficacy of perilla oil, imidacloprid, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS Perilla Oil 1% T 3Imidacloprid 0.005 μg 60 OBS.* CALC.** Perilla Oil + Imidacloprid 1% +0.005 μg  87 ‡ 61.2 Perilla Oil 2% 3 Imidacloprid 0.005 μg 60 OBS.*CALC.** Perilla Oil + Imidacloprid 2% + 0.005 μg 100 ‡ 61.2 T 3%efficacy was derived from data that underwent probit analysis to predictlethal dose values from topical application bioassay. *Obs. = observedefficacy **Calc. = efficacy calculated using Colby (1967) formula ‡Since the actual insecticidal kill rate exceeds the calculated value,then the action of the combination is super-additive or a synergisticeffect is present.

TABLE 60 Efficacy of β-caryophyllene, imidacloprid, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS β-caryophyllene 3% 50Imidacloprid 0.005 μg 50 OBS.* CALC.** β-caryophyllene + Imidacloprid3% + 0.005 μg 100‡ 75 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 61 Efficacy of farnesene, imidacloprid, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS Farnesene 3% 7Imidacloprid 0.005 μg 53 OBS.* CALC.** Farnesene + Imidacloprid 3% +0.005 μg 100‡ 56.29 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 62 Efficacy of linolenic acid, imidacloprid, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS Linolenic Acid 3% 13Imidacloprid 0.005 μg 53 OBS.* CALC.** Linolenic Acid + Imidacloprid3% + 0.005 μg 100‡ 59.11 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 63 Efficacy of D-limonene, Imidacloprid, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS D-limonene 5% 23Imidacloprid 0.005 μg 43 OBS.* CALC.** D-limonene + Imidacloprid 5% +0.005 μg 97‡ 56.11 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 64 Efficacy of (R)-(−)-Carvone, Imidacloprid, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS (R)-(−)-Carvone 3% 23Imidacloprid 0.005 μg 43 OBS.* CALC.** (R)-(−)-Carvone + Imidacloprid3% + 0.005 μg 93‡ 56.11 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 65 Efficacy of (S)-(+)-Carvone, Imidacloprid, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS (S)-(+)-Carvone 3% 20Imidacloprid 0.005 μg 53 OBS.* CALC.** (S)-(+)-Carvone + Imidacloprid3% + 0.005 μg 100‡ 62.4 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 66 Efficacy of (1R)-(−)-Myrtenal, Imidacloprid, and a combinationof both against adult, virgin, female Aedes aegypti mosquitoes. CONCEN-% MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS (1R)-(−)-Myrtenal 2%47 Imidacloprid 0.005 μg 53 OBS.* CALC.** (1R)-(−)-Myrtenal +Imidacloprid 2% + 0.005 μg 90‡ 75.09 *Obs. = observed efficacy **Calc. =efficacy calculated using Colby (1967) formula ‡Since the actualinsecticidal kill rate exceeds the calculated value, then the action ofthe combination is super-additive or a synergistic effect is present.

TABLE 67 Efficacy of (S)-(−)-Perillyl alcohol, Imidacloprid, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS(S)-(−)-Perillyl alcohol 2% 47 Imidacloprid 0.005 μg 53 OBS.* CALC.**(S)-(−)-Perillyl alcohol + 2% + 0.005 μg 97‡ 75.09 Imidacloprid *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 68 Efficacy of (S)-(−)-Perillic acid, Imidacloprid, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS(S)-(−)-Perillic acid 1% 13 Imidacloprid 0.005 μg 53 OBS.* CALC.**(S)-(−)-Perillic acid + 1% + 0.005 μg 83‡ 59.11 Imidacloprid *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

Example 39

Perilla oil and various perilla oil components, various perillaldehydeanalogs, and insecticides were tested against mosquitoes as detailed inReference Example 1 with results show in Tables 69-75.

TABLE 69 Efficacy of Perilla oil, Permethrin, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS Perilla oil 2% 3Permethrin 0.0003 μg 27 OBS.* CALC.** Perilla oil + Permethrin 2% +0.0003 μg 53‡ 29.19 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 70 Efficacy of D-limonene, Permethrin, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS D-limonene 5% 47Permethrin 0.0003 μg 17 OBS.* CALC.** D-limonene + Permethrin 5% +0.0003 μg 53‡ 56.01 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate does not exceed the calculated value, then the action of thecombination is not super-additive or synergistic.

TABLE 71 Efficacy of (R)-(−)-Carvone, Permethrin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS (R)-(−)-Carvone 3% 33Permethrin 0.0003 μg 17 OBS.* CALC.** (R)-(−)-Carvone + Permethrin 3% +0.0003 μg 60‡ 44.39 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 72 Efficacy of (S)-(+)-Carvone, Permethrin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS (S)-(+)-Carvone 3% 20Permethrin 0.0003 μg 17 OBS.* CALC.** (S)-(+)-Carvone + Permethrin 3% +0.0003 μg 67‡ 33.6 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 73 Efficacy of (1R)-(−)-Myrtenal, Permethrin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS (1R)-(−)-Myrtenal 2% 47Permethrin 0.0003 μg 17 OBS.* CALC.** (1R)-(−)-Myrtenal + Permethrin2% + 0.0003 μg 43‡ 56.01 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate does not exceed the calculated value, then the action of thecombination is not super-additive or synergistic.

TABLE 74 Efficacy of (S)-(−)-Perillyl alcohol, Permethrin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS(S)-(−)-Perillyl alcohol 2% 47 Permethrin 0.0003 μg 17 OBS.* CALC.**(S)-(−)-Perillyl alcohol + 2% + 0.0003 μg 50‡ 56.01 Permethrin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate does not exceed thecalculated value, then the action of the combination is notsuper-additive or synergistic.

TABLE 75 Efficacy of (S)-(−)-Perillic acid, Permethrin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS(S)-(−)-Perillic acid 1% 13 Permethrin 0.0003 μg 17 OBS.* CALC.**(S)-(−)-Perillic acid + 1% + 0.0003 μg 100‡ 27.79 Permethrin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

Example 40

Perilla oil and various perilla oil components, various perillaldehydeanalogs, and insecticides were tested against mosquitoes as detailed inReference Example 1 with results show in Tables 76-86.

TABLE 76 Efficacy of Perilla oil, Sumithrin, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS Perilla oil 3% 20Sumithrin 0.0007 μg 27 OBS.* CALC.** Perilla oil + Sumithrin 3% + 0.0007μg 57 ‡ 41.6 Perilla oil 4% 17 Sumithrin 0.0007 μg 27 OBS.* CALC.**Perilla oil + Sumithrin 4% + 0.0007 μg 80 ‡ 39.41 Perilla oil 5% 37Sumithrin 0.0007 μg 27 OBS.* CALC.** Perilla oil + Sumithrin 5% + 0.0007μg 77 ‡ 54.01 Perilla oil 6% 50 Sumithrin 0.0007 μg 27 OBS.* CALC.**Perilla oil + Sumithrin 6% + 0.0007 μg 93 ‡ 63.5 *Obs. = observedefficacy **Calc. = efficacy calculated using Colby (1967) formula ‡Since the actual insecticidal kill rate exceeds the calculated value,then the action of the combination is super-additive or a synergisticeffect is present.

TABLE 77 Efficacy of Perillaldehyde, Sumithrin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS Perillaldehyde 2% 57Sumithrin 0.0007 μg 40 OBS.* CALC.** Perillaldehyde + Sumithrin 2% +0.0007 μg 70 ‡ 74.2 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡ Since the actual insecticidalkill rate does not exceed the calculated value, then the action of thecombination is not super-additive or synergistic.

TABLE 78 Efficacy of Farnesene, Sumithrin, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS Farnesene 3% 7Sumithrin 0.0007 μg 40 OBS.* CALC.** Perillaldehyde + Sumithrin 3% +0.0007 μg 80 ‡ 44.2 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡ Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 79 Efficacy of Linolenic acid, Sumithrin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS Linolenic acid 3% 0Sumithrin 0.0007 μg 40 OBS.* CALC.** Linolenic acid + Sumithrin 3% +0.0007 μg 13 ‡ 40 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡ Since the actual insecticidalkill rate does not exceed the calculated value, then the action of thecombination is not super-additive or synergistic.

TABLE 80 Efficacy of β-Caryophyllene, Sumithrin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS β-Caryophyllene 3% 0Sumithrin 0.0007 μg 40 OBS.* CALC.** β-Caryophyllene + Sumithrin 3% +0.0007 μg 83‡ 40 *Obs. = observed efficacy **Calc. = efficacy calculatedusing Colby (1967) formula ‡Since the actual insecticidal kill rateexceeds the calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

TABLE 81 Efficacy of D-limonene, Sumithrin, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS D-limonene 5% 57Sumithrin 0.0007 μg 40 OBS.* CALC.** D-limonene + Sumithrin 5% + 0.0007μg 93‡ 74.2 *Obs. = observed efficacy **Calc. = efficacy calculatedusing Colby (1967) formula ‡Since the actual insecticidal kill rateexceeds the calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

TABLE 82 Efficacy of (R)-(−)-Carvone, Sumithrin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS (R)-(−)-Carvone 3% 20Sumithrin 0.0007 μg 40 OBS.* CALC.** (R)-(−)-Carvone + 3% + 0.0007 μg73_(‡) 52 Sumithrin *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡)Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 83 Efficacy of (S)-(+)-Carvone, Sumithrin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS (S)-(+)-Carvone 3% 10Sumithrin 0.0007 μg 40 OBS.* CALC.** (S)-(+)-Carvone + 3% + 0.0007 μg97_(‡) 46 Sumithrin *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡)Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 84 Efficacy of (1R)-(−)-Myrtenal, Sumithrin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS (1R)-(−)-Myrtenal 2% 3Sumithrin 0.0007 μg 40 OBS.* CALC.** (1R)-(−)-Myrtenal + 2% + 0.0007 μg67_(‡) 41.8 Sumithrin *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡)Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 85 Efficacy of (S)-(−)-Perillyl alcohol, Sumithrin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS(S)-(−)-Perillyl alcohol 2% 70 Sumithrin 0.0007 μg 40 OBS.* CALC.**(S)-(−)-Perillyl alcohol + 2% + 0.0007 μg 77_(‡) 82 Sumithrin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate does not exceed thecalculated value, then the action of the combination is notsuper-additive or synergistic.

TABLE 86 Efficacy of (S)-(−)-Perillic acid, Sumithrin, and a combinationof both against adult, virgin, female Aedes aegypti mosquitoes. %MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS (S)-(−)-Perillicacid 1% 87 Sumithrin 0.0007 μg 40 OBS.* CALC.** (S)-(−)-Perillic acid +1% + 0.0007 μg 27_(‡) 92.2 Sumithrin *Obs. = observed efficacy **Calc. =efficacy calculated using Colby (1967) formula _(‡)Since the actualinsecticidal kill rate does not exceed the calculated value, then theaction of the combination is not super-additive or synergistic.

Example 41

Perilla oil and various perilla oil components, various perillaldehydeanalogs, and insecticides were tested against mosquitoes as detailed inReference Example 1 with results show in Tables 87-97.

TABLE 87 Efficacy of Perilla oil, Prallethrin, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Perilla oil 1%  3Prallethrin 0.00075 μg 37 OBS.* CALC.** Perilla oil + Prallethrin 1% +0.00075 μg  97_(‡) 38.89 Perilla oil 2% 13 Prallethrin 0.00075 μg 37OBS.* CALC.** Perilla oil + Prallethrin 2% + 0.00075 μg 100_(‡) 45.19Perilla oil 3% 13 Prallethrin 0.00075 μg 37 OBS.* CALC.** Perilla oil +Prallethrin 3% + 0.00075 μg 100_(‡) 45.19 Perilla oil 4% 40 Prallethrin0.00075 μg 37 OBS.* CALC.** Perilla oil + Prallethrin 4% + 0.00075 μg100_(‡) 62.2  Perilla oil 5% 63 Prallethrin 0.00075 μg 37 OBS.* CALC.**Perilla oil + Prallethrin 5% + 0.00075 μg 100_(‡) 76.69 *Obs. = observedefficacy **Calc. = efficacy calculated using Colby (1967) formula_(‡)Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 88 Efficacy of Perillaldehyde, Prallethrin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Perillaldehyde 1%  3Prallethrin 0.00075 μg 37 OBS.* CALC.** Perillaldehyde + Prallethrin1% + 0.00075 μg 47_(‡) 38.89 Perillaldehyde 2% 60 Prallethrin 0.00075 μg37 OBS.* CALC.** Perillaldehyde + Prallethrin 2% + 0.00075 μg 77_(‡)74.8  Perillaldehyde 3% 97 Prallethrin 0.00075 μg 37 OBS.* CALC.**Perillaldehyde + Prallethrin 3% + 0.00075 μg 90_(§) 98.11 *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present. _(§)Since the actual insecticidalkill rate does not exceed the calculated value, then the action of thecombination is not super-additive or synergistic.

TABLE 89 Efficacy of Farnasene, Prallethrin, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Farnasene 3%  7 Prallethrin0.00075 μg 20 OBS.* CALC.** Farnasene + Prallethrin 3% + 0.00075 μg90_(‡) 25.6 *Obs. = observed efficacy **Calc. = efficacy calculatedusing Colby (1967) formula _(‡)Since the actual insecticidal kill rateexceeds the calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

TABLE 90 Efficacy of Linolenic acid, Prallethrin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Linolenic acid 3%  0Prallethrin 0.00075 μg 20 OBS.* CALC.** Linolenic acid + Prallethrin3% + 0.00075 μg 7_(‡) 20 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡)Since the actual insecticidalkill rate does not exceed the calculated value, then the action of thecombination is not super-additive or synergistic.

TABLE 91 Efficacy of β-Caryophyllene, Prallethrin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS β-Caryophyllene 3% 0Prallethrin 0.00075 μg 20 OBS.* CALC.** β-Caryophyllene + 3% + 0.00075μg 33_(‡) 20 Prallethrin *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡)Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 92 Efficacy of D-limonene, Prallethrin, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS D-limonene 5% 7 Prallethrin0.00075 μg 20 OBS.* CALC.** D-limonene + 5% + 0.00075 μg 77_(‡) 25.6Prallethrin *Obs. = observed efficacy **Calc. = efficacy calculatedusing Colby (1967) formula _(‡)Since the actual insecticidal kill rateexceeds the calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

TABLE 93 Efficacy of (R)-(−)-Carvone, Prallethrin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS (R)-(−)-Carvone 3% 3Prallethrin 0.00075 μg 20 OBS.* CALC.** (R)-(−)-Carvone + 3% + 0.00075μg 70_(‡) 22.4 Prallethrin *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡)Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 94 Efficacy of (S)-(+)-Carvone, Prallethrin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS (S)-(+)-Carvone 3% 10Prallethrin 0.00075 μg 20 OBS.* CALC.** (S)-(+)-Carvone + 3% + 0.00075μg 73_(‡) 28 Prallethrin *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡)Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 95 Efficacy of (1 R)-(−)-Myrtenal, Prallethrin, and a combinationof both against adult, virgin, female Aedes aegypti mosquitoes. ACTIVEINGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS (1R)-(−)-Myrtenal 2% 0 Prallethrin 0.00075 μg 20 OBS.* CALC.** (1R)-(−)-Myrtenal +Prallethrin 2% + 0.00075 μg 3 _(‡) 20 *Obs. = observed efficacy **Calc.= efficacy calculated using Colby (1967) formula _(‡) Since the actualinsecticidal kill rate does not exceed the calculated value, then theaction of the combination is not super-additive or synergistic.

TABLE 96 Efficacy of (S)-(−)-Perillyl alcohol, Prallethrin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS(S)-(−)-Perillyl alcohol 2% 3 Prallethrin 0.00075 μg 20 OBS.* CALC.**(S)-(−)-Perillyl alcohol + 2% + 0.00075 μg 87_(‡) 22.4 Prallethrin *Obs.= observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 97 Efficacy of (S)-(−)-Perillic acid, Prallethrin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS(S)-(−)-Perillic acid 1% 7 Prallethrin 0.00075 μg 20 OBS.* CALC.**(S)-(−)-Perillic acid + 1% + 0.00075 μg 93_(‡) 25.6 Prallethrin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

Example 42

Various perillaldehyde analogs, and insecticides were tested againstmosquitoes as detailed in Reference Example 1 with results show inTables 98-103.

TABLE 98 Efficacy of D-limonene, Etofenprox, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. ACTIVEINGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS D-limonene 5% 13Etofenprox 0.002 μg 37 OBS.* CALC.** D-limonene + Etofenprox 5% + 0.002μg 93 _(‡) 45.19 *Obs. = observed efficacy **Calc. = efficacy calculatedusing Colby (1967) formula ‡ Since the actual insecticidal kill rateexceeds the calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

TABLE 99 Efficacy of (R)-(−)-Carvone, Etofenprox, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. ACTIVEINGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS (R)-(−)-Carvone 3% 13Etofenprox 0.002 μg 37 OBS.* CALC.** (R)-(−)-Carvone + Etofenprox 3% +0.002 μg 90 _(‡) 45.19 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡)Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 100 Efficacy of (S)-(+)-Carvone, Etofenprox, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. ACTIVEINGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS (S)-(+)-Carvone 3%  7Etofenprox 0.002 μg 37 OBS.* CALC.** (S)-(+)-Carvone + Etofenprox 3% +0.002 μg 70 _(‡) 41.41 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡) Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 101 Efficacy of (1R)-(−)-Myrtenal, Etofenprox, and a combinationof both against adult, virgin, female Aedes aegypti mosquitoes. ACTIVEINGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS (1R)-(−)-Myrtenal 2%43 Etofenprox 0.002 μg 37 OBS.* CALC.** (1R)-(−)-Myrtenal + Etofenprox2% + 0.002 μg 97 _(‡) 64.09 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡) Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 102 Efficacy of (S)-(−)-Perillyl alcohol, Etofenprox, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. ACTIVE INGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS(S)-(−)-Perillyl alcohol 2% 80 Etofenprox 0.002 μg 37 OBS.* CALC.**(S)-(−)-Perillyl alcohol + Etofenprox 2% + 0.002 μg 100 _(‡) 87.4 *Obs.= observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡) Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 103 Efficacy of (S)-(−)-Perillic acid, Etofenprox, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. ACTIVE INGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS(S)-(−)-Perillic acid 1% 63 Etofenprox 0.002 μg 37 OBS.* CALC.**(S)-(−)-Perillic acid + Etofenprox 1% + 0.002 μg 93_(‡) 76.69 *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

Example 43

Perilla oil and various perillaldehyde analogs, and insecticides weretested against mosquitoes as detailed in Reference Example 1 withresults show in Tables 104-110.

TABLE 104 Efficacy of Perilla oil, Pyrethrins, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. ACTIVEINGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS Perilla oil 1%  3Pyrethrins 0.0015 μg 30 OBS.* CALC.** Perilla oil + Pyrethrins 1% +0.0015 μg 60 _(‡) 32.1 Perilla oil 2% 10 Pyrethrins 0.0015 μg 30 OBS.*CALC.** Perilla oil + Pyrethrins 2% + 0.0015 μg 83 _(‡) 37   Perilla oil3% 23 Pyrethrins 0.0015 μg 30 OBS.* CALC.** Perilla oil + Pyrethrins3% + 0.0015 μg 83 _(‡) 46.1 Perilla oil 4% 53 Pyrethrins 0.0015 μg 30OBS.* CALC.** Perilla oil + Pyrethrins 4% + 0.0015 μg 90 _(‡) 67.1Perilla oil 5% 70 Pyrethrins 0.0015 μg 30 OBS.* CALC.** Perilla oil +Pyrethrins 5% + 0.0015 μg 93 _(‡) 79    *Obs. = observed efficacy**Calc. = efficacy calculated using Colby (1967) formula _(‡) Since theactual insecticidal kill rate exceeds the calculated value, then theaction of the combination is super-additive or a synergistic effect ispresent.

TABLE 105 Efficacy of D-limonene, Pyrethrins, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. ACTIVEINGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS D-limonene 5% 50Pyrethrins 0.0015 μg 53 OBS.* CALC.** D-limonene + Pyrethrins 5% +0.0015 μg 100 _(‡) 76.5 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡) Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 106 Efficacy of (R)-(−)-Carvone, Pyrethrins, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. ACTIVEINGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS (R)-(−)-Carvone 3% 10Pyrethrins 0.0015 μg 53 OBS.* CALC.** (R)-(−)-Carvone + Pyrethrins 3% +0.0015 μg 83 _(‡) 57.7 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡) Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 107 Efficacy of (S)-(+)-Carvone, Pyrethrins, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. ACTIVEINGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS (S)-(+)-Carvone 3% 17Pyrethrins 0.0015 μg 53 OBS.* CALC.** (S)-(+)-Carvone + Pyrethrins 3% +0.0015 μg 70 _(‡) 60.99 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡) Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 108 Efficacy of (1R)-(−)-Myrtenal, Pyrethrins, and a combinationof both against adult, virgin, female Aedes aegypti mosquitoes. ACTIVEINGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS (1R)-(−)-Myrtenal 2%10 Pyrethrins 0.0015 μg 53 OBS.* CALC.** (1R)-(−)-Myrtenal + Pyrethrins2% + 0.0015 μg 77 _(‡) 57.7 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡) Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 109 Efficacy of (S)-(−)-Perillyl alcohol, Pyrethrins, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. ACTIVE INGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS(S)-(−)-Perillyl alcohol 2% 67 Pyrethrins 0.0015 μg 53 OBS.* CALC.**(S)-(−)-Perillyl alcohol + Pyrethrins 2% + 0.0015 μg 93 _(‡) 84.49 *Obs.= observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡) Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 110 Efficacy of (S)-(−)-Perillic acid, Pyrethrins, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. ACTIVE INGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS(S)-(−)-Perillic acid 1% 20 Pyrethrins 0.0015 μg 53 OBS.* CALC.**(S)-(−)-Perillic acid + Pyrethrins 1% + 0.0015 μg 93 _(‡) 62.4 *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡) Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

Example 44

The insecticide spinosad was tested with perilla oil and variousperillaldehyde analogs against mosquitoes as detailed in ReferenceExample 1 with results show in Tables 111-115.

TABLE 111 Efficacy of Perilla oil, Spinosad, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. ACTIVEINGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS Perilla oil 2% 3Spinosad 0.02 μg 33 OBS.* CALC.** Perilla oil + Spinosad 2% + 0.02 μg 43_(‡) 35.01 Perilla oil 3% 7 Spinosad 0.02 μg 33 OBS.* CALC.** Perillaoil + Spinosad 3% + 0.02 μg 93 _(‡) 37.69 Perilla oil 4% 3 Spinosad 0.02μg 33 OBS.* CALC.** Perilla oil + Spinosad 4% + 0.02 μg 93 _(‡) 35.01Perilla oil 5% 40 Spinosad 0.02 μg 33 OBS.* CALC.** Perilla oil +Spinosad 5% + 0.02 μg 97 _(‡) 59.8  *Obs. = observed efficacy **Calc. =efficacy calculated using Colby (1967) formula _(‡) Since the actualinsecticidal kill rate exceeds the calculated value, then the action ofthe combination is super-additive or a synergistic effect is present.

TABLE 112 Efficacy of Perillaldehyde, Spinosad, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. ACTIVEINGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS Perillaldehyde 1%  0Spinosad 0.02 μg 33 OBS.* CALC.** Perillaldehyde + Spinosad 1% + 0.02 μg 7 _(‡) 33 Perillaldehyde 2% 10 Spinosad 0.02 μg 33 OBS.* CALC.**Perillaldehyde + Spinosad 2% + 0.02 μg 20 _(‡) 39.7 Perillaldehyde 3% 73Spinosad 0.02 μg 33 OBS.* CALC.** Perillaldehyde + Spinosad 3% + 0.02 μg63 _(‡) 81.91 *Obs. = observed efficacy **Calc. = efficacy calculatedusing Colby (1967) formula _(‡) Since the actual insecticidal kill rateexceeds the calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

TABLE 113 Efficacy of Farnasene, Spinosad, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. ACTIVEINGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS Farnasene 3%  7Spinosad 0.02 μg 33 OBS.* CALC.** Farnasene + Spinosad 3% + 0.02 μg 40_(‡) 37.69 *Obs. = observed efficacy **Calc. = efficacy calculated usingColby (1967) formula _(‡) Since the actual insecticidal kill rateexceeds the calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

TABLE 114 Efficacy of Linolenic acid, Spinosad, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. ACTIVEINGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS Linolenic acid 3% 10Spinosad 0.02 μg 33 OBS.* CALC.** Linolenic acid + Spinosad 3% + 0.02 μg43 _(‡) 39.7 *Obs. = observed efficacy **Calc. = efficacy calculatedusing Colby (1967) formula _(‡) Since the actual insecticidal kill rateexceeds the calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

TABLE 115 Efficacy of β-Caryophyllene, Spinosad, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. ACTIVEINGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS β-Caryophyllene 3%  7Spinosad 0.02 μg 33 OBS.* CALC.** β-Caryophyllene + Spinosad 3% + 0.02μg 77 _(‡) 37.69 *Obs. = observed efficacy **Calc. = efficacy calculatedusing Colby (1967) formula _(‡) Since the actual insecticidal kill rateexceeds the calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

Example 45

The insecticide dinotefuran was tested with perilla oil analogs againstmosquitoes as detailed in Reference Example 1 with results show inTables 116-126.

TABLE 116 Efficacy of Isophorone, Dinotefuran, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. ACTIVEINGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS Isophorone 3% 30Dinotefuran 0.06 μg 37 OBS.* CALC.** Isophorone + Dinotefuran 3% + 0.06μg 97‡ 55.90 *Obs. = observed efficacy **Calc. = efficacy calculatedusing Colby (1967) formula ‡Since the actual insecticidal kill rateexceeds the calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

TABLE 117 Efficacy of 1-Methyl-1-cyclohexene, Dinotefuran, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. ACTIVE INGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS1-Methyl-1-cyclohexene 3% 10 Dinotefuran 0.06 μg 37 OBS.* CALC.**1-Methyl-1-cyclohexene + Dinotefuran 3% + 0.06 μg 97‡ 43.30 *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 118 Efficacy of 1-tert-Butyl-1-cyclohexene, Dinotefuran, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. ACTIVE INGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS1-tert-Butyl . . . 3% 17 Dinotefuran 0.06 μg 37 OBS.* CALC.**1-tert-Butyl . . . + Dinotefuran 3% + 0.06 μg 37‡ 47.71 *Obs. = observedefficacy **Calc. = efficacy calculated using Colby (1967) formula ‡Sincethe actual insecticidal kill rate exceeds the calculated value, then theaction of the combination is super-additive or a synergistic effect ispresent.

TABLE 119 Efficacy of 3,5-Dimethyl-2-cyclohexen-1-one, Dinotefuran, anda combination of both against adult, virgin, female Aedes aegyptimosquitoes. ACTIVE INGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS3,5-Dimethyl . . . 3% 10 Dinotefuran 0.06 μg 37 OBS.* CALC.**3,5-Dimethyl . . . + Dinotefuran 3% + 0.06 μg 87‡ 43.30 *Obs. = observedefficacy **Calc. = efficacy calculated using Colby (1967) formula ‡Sincethe actual insecticidal kill rate exceeds the calculated value, then theaction of the combination is super-additive or a synergistic effect ispresent.

TABLE 120 Efficacy of 4-Methylcyclohexene, Dinotefuran, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. ACTIVE INGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS4-Methylcyclohexene 3%  0 Dinotefuran 0.06 μg 37 OBS.* CALC.**4-Methylcyclohexene + Dinotefuran 3% + 0.06 μg 57‡ 37.00 *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 121 Efficacy of 7,8-Dihydo-α-ionone, Dinotefuran, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. ACTIVE INGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS7,8-Dihydo-α-ionone 3% 50 Dinotefuran 0.06 μg 10 OBS.* CALC.**7,8-Dihydo-α-ionone + Dinotefuran 3% + 0.06 μg 100‡ 55.00 *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 122 Efficacy of 2,4-Dimethyl-3-cyclohexenecarboxaldehyde,Dinotefuran, and a combination of both against adult, virgin, femaleAedes aegypti mosquitoes. ACTIVE INGREDIENT CONCENTRATION % MORTALITYAFTER 24 HRS 2,4-Dimethyl . . . 3% 37 Dinotefuran 0.06 μg 10 OBS.*CALC.** 2,4-Dimethyl . . . + Dinotefuran 3% + 0.06 μg 100‡ 43.30 *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 123 Efficacy of Trivertal, Dinotefuran, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. ACTIVEINGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS Trivertal 3% 13Dinotefuran 0.06 μg 10 OBS.* CALC.** Trivertal + Dinotefuran 3% + 0.06μg 100‡ 21.70 *Obs. = observed efficacy **Calc. = efficacy calculatedusing Colby (1967) formula ‡Since the actual insecticidal kill rateexceeds the calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

TABLE 124 Efficacy of 3-Cyclohexene-1-methanol, Dinotefuran, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. ACTIVE INGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS3-Cyclohexene-1-m . . . 3% 23 Dinotefuran 0.06 μg 37 OBS.* CALC.**3-Cyclohexene-1-m . . . + Dinotefuran 3% + 0.06 μg 100‡ 51.49 *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 125 Efficacy of Terpinolene, Dinotefuran, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. ACTIVEINGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS Terpinolene 3% 13Dinotefuran 0.06 μg 37 OBS.* CALC.** Terpinolene + Dinotefuran 3% + 0.06μg 87‡ 45.19 *Obs. = observed efficacy **Calc. = efficacy calculatedusing Colby (1967) formula ‡Since the actual insecticidal kill rateexceeds the calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

TABLE 126 Efficacy of Piperonyl Butoxide, Dinotefuran, and a combinationof both against adult, virgin, female Aedes aegypti mosquitoes. %MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS PiperonylButoxide 1% 17 Dinotefuran 0.06 μg 57 OBS.* CALC.** Piperonyl Butoxide +1% + 0.06 μg 100‡ 64.31 Dinotefuran *Obs. = observed efficacy **Calc. =efficacy calculated using Colby (1967) formula ‡Since the actualinsecticidal kill rate exceeds the calculated value, then the action ofthe combination is super-additive or a synergistic effect is present.

Example 46

The insecticide thiamethoxam was tested with perilla oil analogs againstmosquitoes as detailed in Reference Example 1 with results show inTables 127-137.

TABLE 127 Efficacy of Isophorone, Thiamethoxam, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Isophorone 3% 33Thiamethoxam 0.01 μg 7 OBS.* CALC.** Isophorone + 3% + 0.01 μg 67‡ 37.69Thiamethoxam *Obs. = observed efficacy **Calc. = efficacy calculatedusing Colby (1967) formula ‡Since the actual insecticidal kill rateexceeds the calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

TABLE 128 Efficacy of 1-Methyl-1-cyclohexene, Thiamethoxam, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. ACTIVE INGREDIENT CONCENTRATION % MORTALITY AFTER 24 HRS1-Methyl-1 . . . 3%  3 Thiamethoxam 0.02 μg 47 OBS.* CALC.** 1-Methyl-1. . . + Thiamethoxam 3% + 0.02 μg 67‡ 48.59 *Obs. = observed efficacy**Calc. = efficacy calculated using Colby (1967) formula ‡Since theactual insecticidal kill rate exceeds the calculated value, then theaction of the combination is super-additive or a synergistic effect ispresent.

TABLE 129 Efficacy of 1-tert-Butyl-1-cyclohexene, Thiamethoxam, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS1-tert-Butyl . . . 3% 40 Thiamethoxam 0.02 μg 47 OBS.* CALC.**1-tert-Butyl . . . + 3% + 0.02 μg 87‡ 68.2 Thiamethoxam *Obs. = observedefficacy **Calc. = efficacy calculated using Colby (1967) formula ‡Sincethe actual insecticidal kill rate exceeds the calculated value, then theaction of the combination is super-additive or a synergistic effect ispresent.

TABLE 130 Efficacy of 3,5-Dimethyl-2-cyclohexen-1-one, Thiamethoxam, anda combination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS3,5-Dimethyl . . . 3% 37 Thiamethoxam 0.02 μg 47 OBS.* CALC.**3,5-Dimethyl . . . + 3% + 0.02 μg 97‡ 66.61 Thiamethoxam *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 131 Efficacy of 4-Methylcyclohexene, Thiamethoxam, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS4-Methylcyclohexene 3% 0 Thiamethoxam 0.02 μg 47 OBS.* CALC.**4-Methylcyclohexene + 3% + 0.02 μg 57‡ 47.00 Thiamethoxam *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 132 Efficacy of 7,8-Dihydro-α-ionone, Thiamethoxam, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS7,8-Dihydro-α-ionone 3% 53 Thiamethoxam 0.0075 μg 23 OBS.* CALC.**7,8-Dihydro-α-ionone + 3% + 0.0075 μg 87‡ 63.81 Thiamethoxam *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 133 Efficacy of 2,4-Dimethyl-3-cyclohexenecarboxaldehyde,Thiamethoxam, and a combination of both against adult, virgin, femaleAedes aegypti mosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATIONAFTER 24 HRS 2,4-Dimethyl . . . 3% 10 Thiamethoxam 0.0075 μg 23 OBS.*CALC.** 2,4-Dimethyl . . . + 3% + 0.0075 μg 100‡ 30.70 Thiamethoxam*Obs. = observed efficacy **Calc. = efficacy calculated using Colby(1967) formula ‡Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 134 Efficacy of Trivertal, Thiamethoxam, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Trivertal 3% 17Thiamethoxam 0.0075 μg 23 OBS.* CALC.** Trivertal + 3% + 0.0075 μg 90‡36.09 Thiamethoxam *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 135 Efficacy of 3-Cyclohexene-1-methanol, Thiamethoxam, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS3-Cyclohexene-1-m . . . 3% 70 Thiamethoxam 0.02 μg 57 OBS.* CALC.**3-Cyclohexene-1- 3% + 0.02 μg 100‡ 87.1 m . . . + Thiamethoxam *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 136 Efficacy of Terpinolene, Thiamethoxam, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Terpinolene 3% 40Thiamethoxam 0.02 μg 57 OBS.* CALC.** Terpinolene + 3% + 0.02 μg 100‡74.2 Thiamethoxam *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 137 Efficacy of Pipeonyl Butoxide, Thiamethoxam, and a combinationof both against adult, virgin, female Aedes aegypti mosquitoes. %MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS PiperonylButoxide 1% 67 Thiamethoxam 0.02 μg 87 OBS.* CALC.** PiperonylButoxide + 1% + 0.02 μg 97‡ 95.71 Thiamethoxam *Obs. = observed efficacy**Calc. = efficacy calculated using Colby (1967) formula ‡Since theactual insecticidal kill rate exceeds the calculated value, then theaction of the combination is super-additive or a synergistic effect ispresent.

Example 47

The insecticide clothianidin was tested with perilla oil analogs againstmosquitoes as detailed in Reference Example 1 with results show inTables 138-148.

TABLE 138 Efficacy of Isophorone, Clothianidin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Isophorone 3% 60Clothianidin 0.02 μg 43 OBS.* CALC.** Isophorone + 3% + 0.02 μg ‡10077.2 Clothianidin *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 139 Efficacy of 1-Methyl-1-cyclohexene, Clothianidin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS1-Methyl-1-cyclohexene 3% 0 Clothianidin 0.02 μg 43 OBS.* CALC.**1-Methyl-1-cyclohexene + 3% + 0.02 μg ‡ 90 43 Clothianidin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡ Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 140 Efficacy of 1-tert-Butyl-1-cyclohexene, Clothianidin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS1-tert-Butyl . . . 3% 10 Clothianidin 0.02 μg 43 OBS.* CALC.**1-tert-Butyl . . . + 3% + 0.02 μg ‡73 48.7 Clothianidin *Obs. = observedefficacy **Calc. = efficacy calculated using Colby (1967) formula ‡Sincethe actual insecticidal kill rate exceeds the calculated value, then theaction of the combination is super-additive or a synergistic effect ispresent.

TABLE 141 Efficacy of 3,5-Dimethyl-2-cyclohexen-1-one, Clothianidin, anda combination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS3,5-Dimethyl . . . 3% 37 Clothianidin 0.02 μg 43 OBS.* CALC.**3,5-Dimethyl . . . + 3% + 0.02 μg ‡97 64.09 Clothianidin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 142 Efficacy of 4-Methylcyclohexene, Clothianidin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS4-Methylcyclohexene 3% 0 Clothianidin 0.02 μg 43 OBS.* CALC.**4-Methylcyclohexene + 3% + 0.02 μg ‡83 43 Clothianidin *Obs. = observedefficacy **Calc. = efficacy calculated using Colby (1967) formula ‡Sincethe actual insecticidal kill rate exceeds the calculated value, then theaction of the combination is super-additive or a synergistic effect ispresent.

TABLE 143 Efficacy of 7,8-Dihydro-α-ionone, Clothianidin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS7,8-Dihydro-α-ionone 3% 20 Clothianidin 0.02 μg 50 OBS.* CALC.**7,8-Dihydro-α-ionone + 3% + 0.02 μg ‡ 100 60 Clothianidin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡ Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 144 Efficacy of 2,4-Dimethyl-3-cyclohexenecarboxaldehyde,Clothianidin, and a combination of both against adult, virgin, femaleAedes aegypti mosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATIONAFTER 24 HRS 2,4-Dimethyl . . . 3% 27 Clothianidin 0.02 μg 50 OBS.*CALC.** 2,4-Dimethyl . . . + 3% + 0.02 μg ‡ 93 63.5 Clothianidin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡ Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 145 Efficacy of Trivertal, Clothianidin, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS Trivertal 3% 10Clothianidin 0.02 μg 50 OBS.* CALC.** Trivertal + Clothianidin 3% + 0.02μg ‡ 67 55 *Obs. = observed efficacy **Calc. = efficacy calculated usingColby (1967) formula ‡ Since the actual insecticidal kill rate exceedsthe calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

TABLE 146 Efficacy of 3-Cyclohexene-1-methanol, Clothianidin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS3-Cyclohexene-1-m . . . 3% 40 Clothianidin 0.015 μg 0 OBS.* CALC.**3-Cyclohexene-1-m . . . + 3% + 0.015 μg ‡ 100 40 Clothianidin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡ Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 147 Efficacy of Terpinolene, Clothianidin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS Terpinolene 3% 37Clothianidin 0.015 μg 0 OBS.* CALC.** Terpinolene + Clothianidin 3% +0.015 μg ‡ 100 37 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡ Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 148 Efficacy of Piperonyl Butoxide, Clothianidin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRSPiperonyl Butoxide 1% 63 Clothianidin 0.01 μg 47 OBS.* CALC.** PiperonylButoxide + Clothianidin 1% + 0.01 μg ‡ 97 80.39 *Obs. = observedefficacy **Calc. = efficacy calculated using Colby (1967) formula ‡Since the actual insecticidal kill rate exceeds the calculated value,then the action of the combination is super-additive or a synergisticeffect is present.

Example 48

The insecticide imidacloprid was tested with perillaldehyde againstmosquitoes as detailed in Reference Example 1 with results show in Table149.

TABLE 149 Efficacy of perillaldehyde, imidacloprid, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS Perillaldehyde 2% 30Imidacloprid 0.0025 μg 83 OBS.* CALC.** Perillaldehyde + Imidacloprid2% + 0.0025 μg 73‡ 88.1 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate does not exceed the calculated value, then the action of thecombination is not super-additive or synergistic.

Example 49

The insecticide imidacloprid was tested with perilla-oil analogs againstmosquitoes as detailed in Reference Example 1 with results show inTables 150-160.

TABLE 150 Efficacy of Isophorone, Imidacloprid, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS Isophorone 3% 37Imidacloprid 0.005 μg 30 OBS.* CALC.** Isophorone + Imidacloprid 3% +0.005 μg 67‡ 55.9 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 151 Efficacy of 1-Methyl-1-cyclohexene, Imidacloprid, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS1-Methyl-1-cyclohexene 3% 0 Imidacloprid 0.005 μg 30 OBS.* CALC.**1-Methyl-1-cyclohexene + 3% + 0.005 μg 27‡ 30 Imidacloprid *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 152 Efficacy of 1-tert-Butyl-1-cyclohexene, Imidacloprid, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS1-tert-Butyl . . . 3% 40 Imidacloprid 0.005 μg 30 OBS.* CALC.**1-tert-Butyl . . . + Imidacloprid 3% + 0.005 μg 80‡ 58 *Obs. = observedefficacy **Calc. = efficacy calculated using Colby (1967) formula ‡Sincethe actual insecticidal kill rate exceeds the calculated value, then theaction of the combination is super-additive or a synergistic effect ispresent.

TABLE 153 Efficacy of 3,5-Dimethyl-2-cyclohexen-1-one, Imidacloprid, anda combination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS3,5-Dimethyl . . . 3% 40 Imidacloprid 0.005 μg 30 OBS.* CALC.**3,5-Dimethyl . . . + Imidacloprid 3% + 0.005 μg 57‡ 58 *Obs. = observedefficacy **Calc. = efficacy calculated using Colby (1967) formula ‡Sincethe actual insecticidal kill rate exceeds the calculated value, then theaction of the combination is super-additive or a synergistic effect ispresent.

TABLE 154 Efficacy of 4-Methylcyclohexene, Imidacloprid, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS4-Methylcyclohexene 3% 0 Imidacloprid 0.005 μg 30 OBS.* CALC.**4-Methylcyclohexene + 3% + 0.005 μg 53‡ 30 Imidacloprid *Obs. = observedefficacy **Calc. = efficacy calculated using Colby (1967) formula ‡Sincethe actual insecticidal kill rate exceeds the calculated value, then theaction of the combination is super-additive or a synergistic effect ispresent.

TABLE 155 Efficacy of 7,8-Dihydro-α-ionone, Imidacloprid, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS7,8-Dihydro-α-ionone 3% 3 Imidacloprid 0.005 μg 30 OBS.* CALC.**7,8-Dihydro-α-ionone + 3% + 0.005 μg 13‡ 32.1 Imidacloprid *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 156 Efficacy of 2,4-Dimethyl-3-cyclohexenecarboxaldehyde,Imidacloprid, and a combination of both against adult, virgin, femaleAedes aegypti mosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATIONAFTER 24 HRS 2,4-Dimethyl . . . 3% 33 Imidacloprid 0.005 μg 30 OBS.*CALC.** 2,4-Dimethyl . . . + Imidacloprid 3% + 0.005 μg 90‡ 53.1 *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 157 Efficacy of Trivertal, Imidacloprid, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Trivertal 3% 23Imidacloprid 0.005 μg 30 OBS.* CALC.** Trivertal + Imidacloprid 3% +0.005 μg 87‡ 46.1 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 158 Efficacy of 3-Cyclohexene-1-methanol, Imidacloprid, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS3-Cyclohexene-1-m . . . 3% 77 Imidacloprid 0.005 μg 40 OBS.* CALC.**3-Cyclohexene- 3% + 0.005 μg 97‡ 86.2 1-m . . . + Imidacloprid *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 159 Efficacy of Terpinolene, Imidacloprid, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Terpinolene 3% 23Imidacloprid 0.005 μg 40 OBS.* CALC.** Terpinolene + 3% + 0.005 μg 70‡53.8 Imidacloprid *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 160 Efficacy of Piperonyl Butoxide, Imidacloprid, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRSPiperonyl Butoxide 1% 17 Imidacloprid 0.003 μg 23 OBS.* CALC.**Piperonyl Butoxide + 1% + 0.003 μg 100‡ 36.09 Imidacloprid *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

Example 50

The insecticide nitenpyram was tested with perilla oil and variousperillaldehyde analogs against mosquitoes as detailed in ReferenceExample 1 with results show in Tables 161-164.

TABLE 161 Efficacy of Perilla oil, Nitenpyram, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Perilla oil 1% 0 Nitenpyram0.008 μg 53 OBS.* CALC.** Perilla oil + Nitenpyram 1% + 0.008 μg 97_(‡)53 Perilla oil 2% 17 Nitenpyram 0.008 μg 53 OBS.* CALC.** Perilla oil +Nitenpyram 2% + 0.008 μg 97_(‡) 60.99 Perilla oil 3% 60 Nitenpyram 0.008μg 53 OBS.* CALC.** Perilla oil + Nitenpyram 3% + 0.008 μg 100_(‡) 81.2*Obs. = observed efficacy **Calc. = efficacy calculated using Colby(1967) formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 162 Efficacy of Farnasene, Nitenpyram, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Farnasene 3% 7 Nitenpyram0.008 μg 3 OBS.* CALC.** Farnasene + Nitenpyram 3% + 0.008 μg 93_(‡)9.79 *Obs. = observed efficacy **Calc. = efficacy calculated using Colby(1967) formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 163 Efficacy of Linolenic acid, Nitenpyram, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Linolenic acid 3% 13Nitenpyram 0.008 μg 3 OBS.* CALC.** Linolenic acid + 3% + 0.008 μg93_(‡) 15.61 Nitenpyram *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡)Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 164 Efficacy of β-Caryophyllene, Nitenpyram, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS β-Caryophyllene 3% 10Nitenpyram 0.008 μg 53 OBS.* CALC.** β-Caryophyllene + 3% + 0.008 μg83_(‡) 57.7 Nitenpyram *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡)Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

Example 51

The pyrethrins were tested with perilla oil analogs against mosquitoesas detailed in Reference Example 1 with results show in Tables 165-174.

TABLE 165 Efficacy of Isophorone, Pyrethrins, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Isophorone 3% 67 Pyrethrins0.001 μg 30 OBS.* CALC.** Isophorone + Pyrethrins 3% + 0.001 μg 83_(‡)76.9 *Obs. = observed efficacy **Calc. = efficacy calculated using Colby(1967) formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 166 Efficacy of 1-Methyl-1-cyclohexene, Pyrethrins, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS1-Methyl-1-cyclohexene 3% 27 Pyrethrins 0.001 μg 30 OBS.* CALC.**1-Methyl-1- 3% + 0.001 μg 80_(‡) 48.9 cyclohexene + Pyrethrins *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 167 Efficacy of 1-tert-Butyl-1-cyclohexene, Pyrethrins, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS1-tert-Butyl . . . 3% 3 Pyrethrins 0.001 μg 30 OBS.* CALC.**1-tert-Butyl . . . + 3% + 0.001 μg 87_(‡) 32.1 Pyrethrins *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 168 Efficacy of 3,5-Dimethyl-2-cyclohexen-1-one, Pyrethrins, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS3,5-Dimethyl . . . 3% 70 Pyrethrins 0.001 μg 63 OBS.* CALC.**3,5-Dimethyl . . . + 3% + 0.001 μg 97_(‡) 88.9 Pyrethrins *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 169 Efficacy of 4-Methylcyclohexene, Pyrethrins, and a combinationof both against adult, virgin, female Aedes aegypti mosquitoes. %MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS4-Methylcyclohexene 3% 3 Pyrethrins 0.001 μg 63 OBS.* CALC.**4-Methylcyclohexene + 3% + 0.001 μg 80_(‡) 64.11 Pyrethrins *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 170 Efficacy of 7,8-Dihydro-α-ionone, Pyrethrins, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS7,8-Dihydro-α-ionone 3% 63 Pyrethrins 0.001 μg 67 OBS.* CALC.**7,8-Dihydro-α-ionone + 3% + 0.001 μg 77_(‡) 87.79 Pyrethrins *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 171 Efficacy of 2,4-Dimethyl-3-cyclohexenecarboxaldehyde,Pyrethrins, and a combination of both against adult, virgin, femaleAedes aegypti mosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATIONAFTER 24 HRS 2,4-Dimethyl . . . 3% 30 Pyrethrins 0.001 μg 67 OBS.*CALC.** 2,4-Dimethyl . . . + 3% + 0.001 μg 93_(‡) 76.9 Pyrethrins *Obs.= observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 172 Efficacy of Trivertal, Pyrethrins, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Trivertal 3% 43 Pyrethrins0.001 μg 67 OBS.* CALC.** Trivertal + 3% + 0.001 μg 90_(‡) 81.19Pyrethrins *Obs. = observed efficacy **Calc. = efficacy calculated usingColby (1967) formula _(‡)Since the actual insecticidal kill rate exceedsthe calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

TABLE 173 Efficacy of 3-Cyclohexene-1-methanol, Pyrethrins, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS3-Cyclohexene-1-m . . . 3% 47 Pyrethrins 0.001 μg 37 OBS.* CALC.**3-Cyclohexene- 3% + 0.001 μg 87_(‡) 66.61 1-m . . . + Pyrethrins *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 174 Efficacy of Terpinolene, Pyrethrins, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Terpinolene 3% 37Pyrethrins 0.001 μg 37 OBS.* CALC.** Terpinolene + Pyrethrins 3% + 0.001μg 97_(‡) 60.31 *Obs. = observed efficacy **Calc. = efficacy calculatedusing Colby (1967) formula _(‡)Since the actual insecticidal kill rateexceeds the calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

Example 52

The insecticide permethrin was tested with perilla oil analogs againstmosquitoes as detailed in Reference Example 1 with results shown inTables 175-184

TABLE 175 Efficacy of Isophorone, Permethrin, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Isophorone 3% 60 Permethrin0.0004 μg 47 OBS.* CALC.** Isophorone + Permethrin 3% + 0.0004 μg 80_(‡)78.8 *Obs. = observed efficacy **Calc. = efficacy calculated using Colby(1967) formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 176 Efficacy of 1-Methyl-1-cyclohexene, Permethrin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS1-Methyl-1-cyclohexene 3% 10 Permethrin 0.0004 μg 47 OBS.* CALC.**1-Methyl-1- 3% + 0.0004 μg 80_(‡) 52.3 cyclohexene + Permethrin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 177 Efficacy of 1-tert-Butyl-1-cyclohexene, Permethrin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS1-tert-Butyl . . . 3% 47 Permethrin 0.0004 μg 47 OBS.* CALC.**1-tert-Butyl . . . + 3% + 0.0004 μg 93_(‡) 71.91 Permethrin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 178 Efficacy of 3,5-Dimethyl-2-cyclohexen-1-one, Permethrin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS3,5-Dimethyl . . . 3% 57 Permethrin 0.0004 μg 53 OBS.* CALC.**3,5-Dimethyl. . . + 3% + 0.0004 μg 87_(‡) 79.79 Permethrin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 179 Efficacy of 4-Methylcyclohexene, Permethrin, and a combinationof both against adult, virgin, female Aedes aegypti mosquitoes. %MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS4-Methylcyclohexene 3% 3 Permethrin 0.0004 μg 47 OBS.* CALC.**4-Methylcyclohexene + 3% + 0.0004 μg 57_(‡) 48.59 Permethrin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 180 Efficacy of 7,8-Dihydro-α-ionone, Permethrin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS7,8-Dihydro-α-ionone 3% 37 Permethrin 0.0004 μg 53 OBS.* CALC.**7,8-Dihydro-α- 3% + 0.0004 μg 60_(‡) 70.39 ionone + Permethrin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 181 Efficacy of 2,4-Dimethyl-3-cyclohexenecarboxaldehyde,Permethrin, and a combination of both against adult, virgin, femaleAedes aegypti mosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATIONAFTER 24 HRS 2,4-Dimethyl... 3% 47 Permethrin 0.0004 μg 53 OBS.* CALC.**2,4-Dimethyl . . . + 3% + 0.0004 μg 83_(‡) 75.09 Permethrin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 182 Efficacy of Trivertal, Permethrin, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Trivertal 3% 20 Permethrin0.0004 μg 53 OBS.* CALC.** Trivertal + Permethrin 3% + 0.0004 μg 60_(‡)62.4 *Obs. = observed efficacy **Calc. = efficacy calculated using Colby(1967) formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 183 Efficacy of 3-Cyclohexene-1-methanol, Permethrin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS3-Cyclohexene-1- 3% 57 methanol Permethrin 0.0003 μg 37 OBS.* CALC.**3-Cyclohexene-1- 3% + 0.0003 μg 100_(‡) 72.91 methanol + Permethrin*Obs. = observed efficacy **Calc. = efficacy calculated using Colby(1967) formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 184 Efficacy of Terpinolene, Permethrin, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Terpinolene 3% 17Permethrin 0.0003 μg 37 OBS.* CALC.** Terpinolene + 3% + 0.0003 μg97_(‡) 47.71 Permethrin *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡)Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

Example 53

The insecticide etofenprox was tested with perilla oil againstmosquitoes as detailed in Reference Example 1 with results show in Table185.

TABLE 185 Efficacy of Perilla oil, Etofenprox, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Perilla oil 2% 0 Etofenprox0.001 μg 27 OBS.* CALC.** Perilla oil + Etofenprox 2% + 0.001 μg 43_(‡)27 Perilla oil 3% 73 Etofenprox 0.001 μg 40 OBS.* CALC.** Perilla oil +Etofenprox 3% + 0.001 μg 87_(‡) 83.8 *Obs. = observed efficacy **Calc. =efficacy calculated using Colby (1967) formula _(‡)Since the actualinsecticidal kill rate exceeds the calculated value, then the action ofthe combination is super-additive or a synergistic effect is present.

Example 54

The insecticide etofenprox was tested with perilla oil analogs againstmosquitoes as detailed in Reference Example 1 with results show inTables 186-195.

TABLE 186 Efficacy of Isophorone, Etofenprox, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Isophorone 3% 57 Etofenprox0.0007 μg 10 OBS.* CALC.** Isophorone + Etofenprox 3% + 0.0007 μg 97_(‡)61.3 *Obs. = observed efficacy **Calc. = efficacy calculated using Colby(1967) formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 187 Efficacy of 1-Methyl-1-cyclohexane, Etofenprox, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS1-Methyl-1-cyclohexane 3% 3 Etofenprox 0.0007 μg 10 OBS.* CALC.**1-Methyl-1-cyclohexane + 3% + 0.0007 μg 53‡ 12.7 Etofenprox *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 188 Efficacy of 1-tert-Butyl-1-cyclohexene, Etofenprox, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS1-tert-Butyl . . . 3% 7 Etofenprox 0.0007 μg 10 OBS.* CALC.**1-tert-Butyl . . . + 3% + 0.0007 μg 60‡ 16.3 Etofenprox *Obs. = observedefficacy **Calc. = efficacy calculated using Colby (1967) formula ‡Sincethe actual insecticidal kill rate exceeds the calculated value, then theaction of the combination is super-additive or a synergistic effect ispresent.

TABLE 189 Efficacy of 3,5-Dimethyl-2-cyclohexen-1-one, Etofenprox, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS3,5-Dimethyl . . . 3% 33 Etofenprox 0.0007 μg 10 OBS.* CALC.**3,5-Dimethyl . . . + 3% + 0.0007 μg 87‡ 39.7 Etofenprox *Obs. = observedefficacy **Calc. = efficacy calculated using Colby (1967) formula ‡Sincethe actual insecticidal kill rate exceeds the calculated value, then theaction of the combination is super-additive or a synergistic effect ispresent.

TABLE 190 Efficacy of 4-Methylcyclohexene, Etofenprox, and a combinationof both against adult, virgin, female Aedes aegypti mosquitoes. CONCEN-% MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS 4-Methylcyclohexene3% 3 Etofenprox 0.0007 μg 10 OBS.* CALC.** 4-Methylcyclohexene + 3% +0.0007 μg 53‡ 12.7 Etofenprox *Obs. = observed efficacy **Calc. =efficacy calculated using Colby (1967) formula ‡Since the actualinsecticidal kill rate exceeds the calculated value, then the action ofthe combination is super-additive or a synergistic effect is present.

TABLE 191 Efficacy of 7,8-Dihydro-α-ionone, Etofenprox, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS7,8-Dihydro-α-ionone 3% 33 Etofenprox 0.0007 μg 10 OBS.* CALC.**7,8-Dihydro-α-ionone + 3% + 0.0007 μg 73‡ 39.7 Etofenprox *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 192 Efficacy of 2,4-Dimethyl-3-cyclohexenecarboxaldehyde,Etofenprox, and a combination of both against adult, virgin, femaleAedes aegypti mosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATIONAFTER 24 HRS 2,4-Dimethyl . . . 3% 23 Etofenprox 0.0007 μg 10 OBS.*CALC.** 2,4-Dimethyl . . . + 3% + 0.0007 μg 17‡ 30.7 Etofenprox *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 193 Efficacy of Trivertal, Etofenprox, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS Trivertal 3% 20Etofenprox 0.0007 μg 10 OBS.* CALC.** Trivertal + Etofenprox 3% + 0.0007μg 70‡ 28 *Obs. = observed efficacy **Calc. = efficacy calculated usingColby (1967) formula ‡Since the actual insecticidal kill rate exceedsthe calculated value, then the action of the combination issuper-additive or a synergistic effect is present.

TABLE 194 Efficacy of 3-Cyclohexene-1-methanol, Etofenprox, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS3-Cyclohexene-1-m . . . 3% 47 Etofenprox 0.0007 μg 3 OBS.* CALC.**3-Cyclohexene-1-m . . . + 3% + 0.0007 μg 93‡ 48.59 Etofenprox *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 195 Efficacy of Terpinolene, Etofenprox, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS Terpinolene 3% 37Etofenprox 0.0007 μg 3 OBS.* CALC.** Terpinolene + Etofenprox 3% +0.0007 μg 77‡ 38.89 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

Example 55

The insecticide sumithrin was tested with perilla oil against mosquitoesas detailed in Reference Example 1 with results show in Table 196.

TABLE 196 Efficacy of Perilla oil, Sumithrin, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS Perilla oil 3% 20Sumithrin 0.0007 μg 27 OBS.* CALC.** Perilla oil + Sumithrin 3% + 0.0007μg 57 ‡ 41.6 Perilla oil 4% 17 Sumithrin 0.0007 μg 27 OBS.* CALC.**Perilla oil + Sumithrin 4% + 0.0007 μg 80 ‡ 39.41 Perilla oil 5% 37Sumithrin 0.0007 μg 27 OBS.* CALC.** Perilla oil + Sumithrin 5% + 0.0007μg 77 ‡ 54.01 Perilla oil 6% 50 Sumithrin 0.0007 μg 27 OBS.* CALC.**Perilla oil + Sumithrin 6% + 0.0007 μg 93 ‡ 63.5 *Obs. = observedefficacy **Calc. = efficacy calculated using Colby (1967) formula ‡Since the actual insecticidal kill rate exceeds the calculated value,then the action of the combination is super-additive or a synergisticeffect is present.

Example 56

The insecticide sumithrin was tested with perilla oil analogs againstmosquitoes as detailed in Reference Example 1 with results show inTables 197-206.

TABLE 197 Efficacy of Isophorone, Sumithrin, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. CONCEN- %MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS Isophorone 3% 30Sumithrin 0.0007 μg 43 OBS.* CALC.** Isophorone acid + 3% + 0.0007 μg90‡ 60.1 Sumithrin *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula ‡Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 198 Efficacy of 1-Methyl-1-cyclohexene, Sumithrin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS1-Methyl-1-cyclohexene 3% 7 Sumithrin 0.0007 μg 43 OBS.* CALC.**1-Methyl-1-cyclohexene + 3% + 0.0007 μg 83‡ 46.99 Sumithrin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula ‡Since the actual insecticidal kill rate exceeds the calculatedvalue, then the action of the combination is super-additive or asynergistic effect is present.

TABLE 199 Efficacy of 1-tert-Butyl-1-cyclohexene, Sumithrin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS1-tert-Butyl . . . 3% 47 Sumithrin 0.0007 μg 43 OBS.* CALC.**1-tert-Butyl . . . + 3% + 0.0007 μg 87‡ 69.79 Sumithrin *Obs. = observedefficacy **Calc. = efficacy calculated using Colby (1967) formula ‡Sincethe actual insecticidal kill rate exceeds the calculated value, then theaction of the combination is super-additive or a synergistic effect ispresent.

TABLE 200 Efficacy of 3,5-Dimethyl-2-cyclohexen-1-one, Sumithrin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS3,5-Dimethyl . . . 3% 63 Sumithrin 0.0007 μg 43 OBS.* CALC.**3,5-Dimethyl . . . + 3% + 0.0007 μg 93_(‡) 78.91 Sumithrin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡) Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 201 Efficacy of 4-Methylcyclohexene, Sumithrin, and a combinationof both against adult, virgin, female Aedes aegypti mosquitoes. %MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS4-Methylcyclohexene 3% 0 Sumithrin 0.0007 μg 43 OBS.* CALC.**4-Methylcyclohexene + 3% + 0.0007 μg 67_(‡) 43 Sumithrin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 202 Efficacy of 7,8-Dihydro-α-ionone, Sumithrin, and a combinationof both against adult, virgin, female Aedes aegypti mosquitoes. CONCEN-% MORTALITY ACTIVE INGREDIENT TRATION AFTER 24 HRS 7,8-Dihydro-α-ionone3% 3 Sumithrin 0.0007 μg 43 OBS.* CALC.** 7,8-Dihydro-α-ionone + 3% +0.0007 μg 97‡ 44.71 Sumithrin *Obs. = observed efficacy **Calc. =efficacy calculated using Colby (1967) formula ‡Since the actualinsecticidal kill rate exceeds the calculated value, then the action ofthe combination is super-additive or a synergistic effect is present.

TABLE 203 Efficacy of 2,4-Dimethyl-3-cyclohexenecarboxaldehyde,Sumithrin, and a combination of both against adult, virgin, female Aedesaegypti mosquitoes. CONCEN- % MORTALITY ACTIVE INGREDIENT TRATION AFTER24 HRS 2,4-Dimethyl . . . 3% 47 Sumithrin 0.0007 μg 43 OBS.* CALC.**2,4-Dimethyl . . . + 3% + 0.0007 μg 47‡ 69.79 Sumithrin *Obs. = observedefficacy **Calc. = efficacy calculated using Colby (1967) formula ‡Sincethe actual insecticidal kill rate does not exceed the calculated value,then the action of the combination is not super-additive or synergistic.

TABLE 204 Efficacy of Trivertal, Sumithrin, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Trivertal 3% 40 Sumithrin0.0007 μg 43 OBS.* CALC.** Trivertal + Sumithrin 3% + 0.0007 μg 37_(‡)65.8 *Obs. = observed efficacy **Calc. = efficacy calculated using Colby(1967) formula _(‡)Since the actual insecticidal kill rate does notexceed the calculated value, then the action of the combination is notsuper-additive or synergistic.

TABLE 205 Efficacy of 3-Cyclohexene-1-methanol, Sumithrin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS3-Cyclohexene-1- 3% 50 methanol Sumithrin 0.0003 μg 27 OBS.* CALC.**3-Cyclohexene-1- 3% + 0.0003 μg 90‡ 63.5 methanol + Sumithrin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 206 Efficacy of Terpinolene, Sumithrin, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Terpinolene 3% 20 Sumithrin0.0003 μg 27 OBS.* CALC.** Terpinolene + Sumithrin 3% + 0.0003 μg 67‡41.6 *Obs. = observed efficacy **Calc. = efficacy calculated using Colby(1967) formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present..

Example 57

The insecticide prallethrin was tested with perilla oil analogs againstmosquitoes as detailed in Reference Example 1 with results show inTables 207-216.

TABLE 207 Efficacy of Isophorone, Prallethrin, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Isophorone 3% 57Prallethrin 0.0005 μg 37 OBS.* CALC.** Isophorone + Prallethrin 3% +0.0005 μg 97_(‡) 72.91 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡)Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

TABLE 208 Efficacy of 1-Methyl-1-cyclohexene, Prallethrin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS1-Methyl-1-cyclohexene 3% 40 Prallethrin 0.0005 μg 37 OBS.* CALC.**1-Methyl-1- 3% + 0.0005 μg 97_(‡) 62.2 cyclohexene + Prallethrin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 209 Efficacy of 1-tert-Butyl-1-cyclohexene, Prallethrin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS1-tert-Butyl . . . 3% 30 Prallethrin 0.0005 μg 37 OBS.* CALC.**1-tert-Butyl . . . + 3% + 0.0005 μg 77_(‡) 55.9 Prallethrin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 210 Efficacy of 3,5-Dimethyl-2-cyclohexen-1one, Prallethrin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS3.5-Dimethyl . . . 3% 30 Prallethrin 0.0005 μg 37 OBS.* CALC.**3,5-Dimethyl . . . + 3% + 0.0005 μg 90_(‡) 55.9 Prallethrin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 211 Efficacy of 4-Methylcyclohexene, Prallethrin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS4-Methylcyclohexene 3% 0 Prallethrin 0.0005 μg 37 OBS.* CALC.**4-Methylcyclohexene + 3% + 0.0005 μg 57_(‡) 37 Prallethrin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 212 Efficacy of 7,8-Dihydro-α-ionone, Prallethrin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS7,8-Dihydro-α-ionone 3% 47 Prallethrin 0.0005 μg 37 OBS.* CALC.**7,8-Dihydro-α-ionone + 3% + 0.0005 μg 97_(‡) 66.61 Prallethrin *Obs. =observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 213 Efficacy of 2,4-Dimethyl-3-cyclohexenecarboxaldehyde,Prallethrin, and a combination of both against adult, virgin, femaleAedes aegypti mosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATIONAFTER 24 HRS 2,4-Dimethyl . . . 3% 13 Prallethrin 0.0005 μg 60 OBS.*CALC.** 2,4-Dimethyl . . . + 3% + 0.0005 μg 77_(‡) 65.2 Prallethrin*Obs. = observed efficacy **Calc. = efficacy calculated using Colby(1967) formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 214 Efficacy of Trivertal, Prallethrin, and a combination of bothagainst adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Trivertal 3% 0 Prallethrin0.0005 μg 60 OBS.* CALC.** Trivertal + Prallethrin 3% + 0.0005 μg 90_(‡)60 *Obs. = observed efficacy **Calc. = efficacy calculated using Colby(1967) formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 215 Efficacy of 3-Cyclohexene-1-methanol, Prallethrin, and acombination of both against adult, virgin, female Aedes aegyptimosquitoes. % MORTALITY ACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS3-Cyclohexene-1- 3% 7 methanol Prallethrin 0.0004 μg 40 OBS.* CALC.**3-Cyclohexene- 3% + 0.0004 μg 87_(‡) 44.2 1-methanol + Prallethrin *Obs.= observed efficacy **Calc. = efficacy calculated using Colby (1967)formula _(‡)Since the actual insecticidal kill rate exceeds thecalculated value, then the action of the combination is super-additiveor a synergistic effect is present.

TABLE 216 Efficacy of Terpinolene, Prallethrin, and a combination ofboth against adult, virgin, female Aedes aegypti mosquitoes. % MORTALITYACTIVE INGREDIENT CONCENTRATION AFTER 24 HRS Terpinolene 3% 20Prallethrin 0.0003 μg 7 OBS.* CALC.** Terpinolene + Prallethrin 3% +0.0003 μg 93_(‡) 25.6 *Obs. = observed efficacy **Calc. = efficacycalculated using Colby (1967) formula _(‡)Since the actual insecticidalkill rate exceeds the calculated value, then the action of thecombination is super-additive or a synergistic effect is present.

Example 58 Open field caged mosquito efficacy study

A formulation including 5% pyrethrin, 7% perilla oil, and 67% Mineraloil was tested to determine the potential efficacy against adult femalemosquitoes in an open field caged study. Spray cages were placed on5-foot stakes, 1 cage per stake, and at an angle parallel to the sprayline. Stakes were placed at 100, 200 and 300 feet down-wind at a 90angle from the spray line. Cages were placed in three rows 100 feetapart. See FIG. 1. A total of 10 spray cages (9 treated and 1 untreatedcontrol) were used in each replicate. 20-25 adult female Aedes aegyptimosquitoes were placed in the cylindrical spray cages. The formulationwas applied at an application rate of 0.53 oz/acre to the area.

Two replicate experiments were conducted. For each replicate, DropletVMDs were 13-15 microns, Drop Densities at all distances were +300/cm²,the air temperature was 79° F., and the winds were consistent from theEast at 6-8 mph. After 1 h, 12 h, and 24 h, the knockdown or mortalitywas calculated as a percent of the total number of mosquitoes for thatreplicate and distance. Results are shown in Table 217.

TABLE 217 1 h 12 h 24 h Distance from spray line knockdown knockdownMortality Replicate 1 100 feet 100% 100% 100% 200 feet 100% 100% 100%300 feet 100% 100% 100% Replicate 2 100 feet 98% 99% 99.9%  200 feet100% 100%  99% 300 feet 100% 100% 99.9% 

Example 59 P450 Activity Assay

Cytochrome P450 enzyme solution was prepared by homogenizing 15, 3 to 5day old, A. aegypti females and centrifuging the mixture at 10,000 g for1 minute. The pellet was discarded, and the supernatant was used as theP450 enzyme stock solution. 10 μL of this P450 enzyme stock and 90 μL of7-ethoxycoumarin solution (0.526 mM of 7-ethoxycoumarin, 1.11 mM NADPH,0.05 mM phosphate buffer) was added to each well of the micropipetteplate to begin the reaction. During the reaction, the micropipette platewas covered with aluminum foil to prevent photo-bleaching. The reactionwas incubated at 30° C. for 4 hours. The reaction was stopped by adding30 μL of stop solution (0.1 mM glycine, pH 10.4, 50% ethanol). Themicropipette plate was then analyzed by measuring the fluorescence(Emission=460 nM, Excitation=360 nM) of each well. High fluorescence wasdirectly related to product, and thus indicated a high level of P450activity. Conversely, low fluorescence indicated less product andsuggested low P450 activity (inhibition).

Measurement of cytochrome P450 enzyme (P450) activity with and withoutinhibitors are shown in FIG. 2. The control treatment contained acetone.PBO, a known cytochrome p450 inhibitor served as a positive control.Both PBO and perillaldehyde when added to the assay acted as inhibitors.FIG. 2 shows that perillaldehyde at 1% is as potent an inhibitor of P450as PBO at 2%. Perillaldehyde at 10% is a more potent inhibitor of P450than PBO at 2%.

Thus, the disclosure provides, among other things, insecticidalcompositions.

What is claimed is:
 1. An insecticidal composition comprising aninsecticide and an active agent present in an amount of about 1% to 99%by weight of the composition, the active agent selected from the groupconsisting of (i) perilla oil; (ii) a perilla oil component selectedfrom the group consisting of farnesene, perillaldehyde, linolenic acid,caryophyllene, limonene, carvone, perillyl alcohol, perillic acid,pinene, linalool, germacrene, bergamotene, and spathulenol; and (iii) aperillaldehyde analog.
 2. The composition of claim 1, wherein the activeagent comprises perilla oil, perillaldehyde, or carvone, including(R)-carvone or (S)-carvone.
 3. The composition of claim 1, wherein theperillaldehyde analog is a compound of formula (A):

wherein: R¹ is selected from the group consisting of —CH₂OH, —CHO, and—COOR^(a); R² is selected from the group consisting of hydrogen, alkyland alkenyl; R³ is selected from the group consisting of hydrogen andalkyl; R⁴ is hydrogen, or R⁴ and R² are taken together with the atoms towhich they are attached to form an optionally substituted ring; andR^(a) is selected from the group consisting of hydrogen and alkyl. 4.The composition of claim 1, wherein the perillaldehyde analog isselected from the group consisting of limonene including D-limonene,perillyl alcohol including (S)-(−)-perillyl alcohol, perillic acidincluding (S)-(−)-perillic acid, myrtenal including (1R)-(−)-myrtenal,and 3-methyl-1-cyclohexene-1-carboxaldehyde.
 5. The composition of claim1, wherein the insecticide is selected from the group consisting ofpyrethrin, pyrethroid, neonicotinoid, chlofenapyr, ethiprole,sulfoxoflor, carbamates, organophosphates, and organochlorines.
 6. Thecomposition of claim 5, wherein the insecticide comprises one or morenaturally occurring pyrethrins selected from the group consisting ofJasomolin-I, Cinerin-I, Pyrethrin-I, Jasmolin-II, Cinerin-II, andPyrethrin-II.
 7. The composition of claim 5, wherein the insecticidecomprises one or more pyrethroids selected from the group consisting ofetofenprox, permethrin, prallethrin, resmethrin, and sumithrin.
 8. Thecomposition of claim 5, wherein the insecticide comprises one or morecompounds selected from the group consisting of allethrin,alpha-cypermethrin, bifenthrin, beta-cypermethrin, cyfluthrin,cypermethrin, deltamethrin, esfenvalerate, etofenprox,lamdba-cyhalothrin, and zeta-cypermethrin.
 9. The composition of claim5, wherein the insecticide comprises one or more neonicotinoids selectedfrom the group consisting of dinotefuran, acetamiprid, clothianidin,imidacloprid, nitenpyram, thiacloprid, and thiamethoxam.
 10. Thecomposition of claim 9, wherein the insecticide comprises at least oneof clothianidin or imidacloprid.
 11. The composition of claim 1, whereinthe composition is substantially free of piperonyl butoxide.
 12. Thecomposition of claim 1, wherein the composition is substantially free ofN-octyl bicycloheptene dicarboximide.
 13. The composition of claim 1,wherein the composition comprises less than about 95% by weight of theinsecticide.
 14. The composition of claim 1, wherein the compositioncomprises less than about 60% by weight of the insecticide.
 15. Thecomposition of claim 1, wherein the composition further comprisesmineral oil, glycerol, or other diluent that provides viscositymodifying properties.
 16. The composition of claim 1, wherein thecomposition is suitable for application as at least one of an aerosol,fog, mist, spray, ultra low volume spray, or surface contact treatment.17. A method for controlling insects, the method comprising contacting apopulation of insects with an effective amount of the composition ofclaim
 1. 18. The method of claim 17, wherein the insect is a mosquito.19. The method of claim 17, wherein the composition is topically appliedto the population in an amount sufficient to kill at least 25% of thepopulation.
 20. The method of claim 17, wherein the composition istopically applied to the population in an amount sufficient to kill atleast 50% of the population.
 21. The method of claim 17, wherein thecomposition is applied by at least one of an aerosol, mist, fog, spray,vapor, ULV spray, or surface contact treatment.
 22. The method of claim17, wherein the population is exposed to the insecticide so that thecomposition is ingested by the insects sufficient to kill at least 50%of the population.